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making potassium (per) chlorate


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Posted

With the concentric electrodes prepared and ready to go I decided to try a test cell. Since the schedule 80 tube was PVC (instead of CPVC) I used clear PVC for the bottom and lid of the cell in lieu of the expensive CPVC plate. It came together well and machined easily. I have to drill and install ports for flow into and out of the electrode chamber, but the basic form is visible in the photos below.

 

If I glue a short section of PVC pipe in a PVC union and install it in the electrode cell, it allows a means of disconnecting the EC from the RC (reaction chamber).

 

More later...

 

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Unfortunately (or fortunately, depending on how you look at it), I won't be able to work on my electrochemical pursuits for a few weeks due to activities that will take me away from my normal life (I'll be hiking with the scouts for a week, then preparing for and attending the PGI convention). I hope to meet some of you at the convention (look for me at rocket manufacturing, I'll be the middle-aged dude swinging a mallet, occasionally, making 1 pounders). Please come up and introduce yourself.

 

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Posted
Man! I need to get the glasses checked, I thought you said, " I'll be the middle-aged dude swinger with a mullet." :) :)
Posted

Man! I need to get the glasses checked, I thought you said, " I'll be the middle-aged dude swinger with a mullet." 2smile.gif 2smile.gif

 

I keep telling folks (while holding my glasses up), "These things aren't a fashion statement!".

 

The only fish I hope to handle anytime soon, will be trout (golden, brown or rainbow), out of the water and into the pan (Yum!).

Posted
Dave, I read the exact same thing. The weird part is that he probably wouldn't even stand out too much.
Posted

Wow, and I thought my eyes were bad.

 

The PGI is in Wisconsin this year and Mumbles is right, the description of the middle aged guy with a mullet would be a good portion of the Wisconsinites from "Up Nort"

 

When I go to the tavern at the lake I run into people with Mullets, their cigarettes rolled up in their shirt sleeves and old faded tattoo's!

 

But when you can get a frosty 16 oz glass of beer for a buck and a quarter, I'll hang out with middle aged men with mullets any day.

  • 3 weeks later...
Posted

Wow, and I thought my eyes were bad.

 

The PGI is in Wisconsin this year and Mumbles is right, the description of the middle aged guy with a mullet would be a good portion of the Wisconsinites from "Up Nort"

 

When I go to the tavern at the lake I run into people with Mullets, their cigarettes rolled up in their shirt sleeves and old faded tattoo's!

 

But when you can get a frosty 16 oz glass of beer for a buck and a quarter, I'll hang out with middle aged men with mullets any day.

 

 

It seems beer (or alcohol in general) is really easy to come by here in Appleton. There appears to be two or three taverns or pubs per block as you drive through downtown (surprising lack of mullets, though; I mustn't be far enough Nort).

 

I'm itching to get back to the electrochemistry experiments. We all are suffering from IDD (ignition deficit disorder) here in Appleton due to the flood yesterday, and my thoughts are turning to making chlorate again. I'll write more about everything later...

 

 

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Posted (edited)

It seems beer (or alcohol in general) is really easy to come by here in Appleton. There appears to be two or three taverns or pubs per block as you drive through downtown (surprising lack of mullets, though; I mustn't be far enough Nort).

 

I'm itching to get back to the electrochemistry experiments. We all are suffering from IDD (ignition deficit disorder) here in Appleton due to the flood yesterday, and my thoughts are turning to making chlorate again. I'll write more about everything later...

 

 

WSMcool2.gif

 

Well, I'm back but tired. I need to rest up from all that fun 2closedeyes.gif zzzZZZ! I saw lots of excellent fireworks, fed MANY mosquitos, and don't expect we'll go back to Appleton any time soon (not an ideal site for the PGI). I did get to discuss electrochemistry with a few folks and some of them even understood what the heck I was talking about 2blink.gif. Home brew oxidizer enthusiasts are hard to come by, and those who actually follow through and produce more than a lab sample are even rarer (few in number, not undercooked; you bunch of jokerswink2.gif ).

 

As I mentioned before, as soon as I figure out a few details I want to continue my pursuit of the Monster (my high-end continuous chlorate system). The components are coming together but I need to iron out a few design details to optimize the system. I do enjoy the challenges but it would be nice to see it function rather than be a collection of expensive junk laying around 2sad.gif.

 

As I iron out those details I'll post the lessons learned along the way so others can benefit from them. More later...

 

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Oh yeah, I met dagabu there. Nice guy.

Edited by WSM
Posted (edited)

PUTZ!!!

 

:lol:

 

Sorry W, couldn't resist. I met WSM and was really impressed with with his overwhelmingly optimistic personality. It was great to meet my heroes at the PGI convention and be able to be part of a piece of history.

 

Tell Kurt that he's OK too... ;) My kids were following him around like the pied piper they were so impressed with his patience and laid back attitude.

Edited by dagabu
Posted

PUTZ!!!

 

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Sorry W, couldn't resist. I met WSM and was really impressed with with his overwhelmingly optimistic personality. It was great to meet my heroes at the PGI convention and be able to be part of a piece of history.

 

Tell Kurt that he's OK too... wink2.gif My kids were following him around like the pied piper they were so impressed with his patience and laid back attitude.

 

 

MORON!!! biggrin2.gif

 

Wow, it must be contagious! I think I spent the whole week re-attaching names to faces. It really was fun to meet several APC members in person, too.

 

Kurt's laid back attitude comes from his Dad, Roy; the quintessential cool Dad (and a former PGI member,too!).

 

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Posted
I was going to stop by and say hello as well, but it seemed like every time I saw you I had to be running off somewhere.
Posted

I was going to stop by and say hello as well, but it seemed like every time I saw you I had to be running off somewhere.

 

Too bad, it would have been fun to chat. Maybe next time...

 

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  • 2 weeks later...
Posted (edited)

In continuing the concentric electrode cell experiment, I did fill the tubular leads with solder (95:5, tin:antimony) which should help keep the electrically resistant titanium metal from heating too much for the PVDF compression fittings. I also added a PVC lip to the lid with a gap to allow a silicone tube seal to help prevent salt creep around the lid.

 

The first attached photo shows the underside of the EC (electrode chamber) lid with the lip solvent-welded on. The lip is a roughly 1/2" cut from some thinwall, PVC 6" pipe; with a section cut out so a gap will exist to allow the seal. After cutting the section out, I (carefully) use a heat gun to soften the ring so it can be formed into the shape seen in the photo (it becomes rigid again when it cools). I then glued the ring to the lid with a heavy metal weight holding it in position (this was tricky since the ring kept trying to slide around till the PVC cement started to set).

 

The second attached photo shows a similar view but completed with the electrodes reinstalled and the silicone seal mounted. The silicone seal is aquarium air tubing, cut to size and joined with a 1" section, split lengthwise and rolled, then forced in till the ends meet (see the second photo). I put a bead of GE Silicone I RTV around the lip and stick the silicone tube ring to it and let the RTV cure to hold it in place. The last step is to cut a slight chamfer on the top inside wall of the EC tank, so the silicone seal can wedge in when installed. If the seal seems too tight a little grease on the seal will help it slide in.

 

post-9734-128364450507_thumb.jpgpost-9734-128364454135_thumb.jpg

 

I still need to add a vent in the lid for hydrogen and the two side ports (one below the electrodes and one above them) to connect the EC to the RC (reaction chamber) where the active reactants will form the chlorate and circulate back through the RC, before eventually overflowing to the CC (crystalization chamber) where the chlorate drops out in this continuous process. I'll try to get good photos of all these steps so you can follow how this goes. I may yet decide to incorporate the electrodes inside the RC instead of outside (with the external EC) but I want to try it this way first.

 

The idea is to have the EC and the RC (deeper and narrower tanks) run at higher temperatures so the chlorate which forms, stays in solution till it overflows naturally to the CC (shallow, wide and long) where the cell liquor cools and the crystals drop out of solution. The depleated liquor is then pumped back into the RC where separate feeds are plumbed in to inject make-up water and KCl (to replace what's used in the process) and acid to control pH and improve efficiency. The heat of the EC and RC also improve efficiency.

 

(Much) More later...

 

 

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Edited by WSM
Posted

To clarify the continuous system design and descriptions I've given, I've drawn a simple layout:

 

post-9734-12843085093_thumb.jpg

 

In this diagram the red arrows show fluid flow.

The blue line is fluid level in the system.

The light blue hexagons are crystals.

 

The EC (electrode chamber), RC (reaction chamber) and CC (crystallization chamber) are indicated.

 

The progress on the system is quite slow at this point due to many other demands on my time (life does get in the way of fun sometimes 2sad.gif wink2.gif ). I hope to get some of the components together and do some test runs before long. As mentioned before, I'm still deciding whether an external EC or integrating the electrodes inside the RC is the better approach. Any thoughts or questions?

 

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Posted

Hi ,

 

First post on APC. I cannot download any of those pictures so I have to post something.

 

Has anyone considered hanging lots of strings in a Chlorate cell to collect the crystallized Chlorate. Crystals of anything have a tendency to stick to fluffy strings when they are hung in a saturated solution. Just lift out the strings and rub off the harvest and put in again.

 

Frank

Posted (edited)

Hi ,

 

First post on APC. I cannot download any of those pictures so I have to post something.

 

Has anyone considered hanging lots of strings in a Chlorate cell to collect the crystallized Chlorate. Crystals of anything have a tendency to stick to fluffy strings when they are hung in a saturated solution. Just lift out the strings and rub off the harvest and put in again.

 

Frank

 

Hi Frank, Welcome to APC!

 

Rock candy?! After you harvest the chlorate you could use the string for a slow fuse 2smile.gifwhistle.gif .

 

Actually frank, the crystals drop out very well as the system runs and the solution doesn't seem so very saturated (maybe I'm off base here, but I haven't considered saturation points, etc.). I admit, since the system works (salt, water and current in; hydrogen and chlorate out), I haven't questioned it. Maybe we should take a closer look.

 

If you're building a system I can recommend Swede's MMO and titanium electrodes in the Agora section.

 

For the pictures, try the "save as" feature and drop them on your desktop. See if you can open them there. If not, maybe someone more computer savvy than me can help you. Good luck.

 

WSMcool2.gif

Edited by WSM
Posted

Please consider the temperature profile in various places. With the electrode chamber getting hot the circulating part of the reaction chamber will get hot too. With the lower EC to RC pipe coming from midway up the RC then the bottom half of the RC will get almost no heat and it may form crystals there as the solution saturates and the temp stays low. Maybe having the lower pipe from the bottom of the RC to the bottom of the EC will circulate and warm more of the cell liquor.

 

Maybe you could just let crystals form in the bottom of the RC and use a glass tube to syphon them out then do a level and concentration check before restarting.

Posted (edited)

Please consider the temperature profile in various places. With the electrode chamber getting hot the circulating part of the reaction chamber will get hot too. With the lower EC to RC pipe coming from midway up the RC then the bottom half of the RC will get almost no heat and it may form crystals there as the solution saturates and the temp stays low. Maybe having the lower pipe from the bottom of the RC to the bottom of the EC will circulate and warm more of the cell liquor.

 

Maybe you could just let crystals form in the bottom of the RC and use a glass tube to syphon them out then do a level and concentration check before restarting.

 

Hi Arthur,

 

Thank you. Excellent point about low circulation in the bottom section of the RC 2ohmy.gif. I overlooked that portion of the design and missed it completely. Nice catch.

 

That in mind, I'll plumb from the bottom of the RC to the lower port on the EC as you suggest. I plan to insulate all of the connections as well and the EC and RC tanks, if neccessary, to keep developed chlorate in solution till it reaches the CC. The goal is to keep the liquor in the RC and EC at 40 degrees C minimum or higher and in the CC below 30 degrees C.

 

 

As for the second suggestion; if this were a batch system, I agree; but for the continuous system as I envision it, it would be counterproductive 2sad.gif. Now for a chlorate to perchlorate system, that may be just the trick; though I believe having the EC inside the RC would be optimal for a perchlorate cell (unless someone can come up with a great idea for a continuous perchlorate system, that is).

 

Thanks for the input! Keep 'em coming.biggrin2.gif

 

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Edited by WSM
Posted
There is SOOOOOOOOOOOOOOOO much wrong with this video that it isnt worth going into such as the use of non safety matches claiming phosphorous is responsible for the colour the extreme cost and the high likely hood of this not actually working and the likely containment of ammonium chlorate
Posted

i could use a helping hand over here. my pc psu seems to be shutting off on me when i go and use the 5 volt side. as long as i'm not touching the electrode into the electrolyte the readings are fine. however when i do put in the electrodes the power is gone. now i can perform this same thing with the 3 volt side everything is just fine burpin away. whats this mean? also my fan doesn't seem to be working either. i'm pretty sure i've done the wiring right, all readings on my volt meter are perfect...12v reads 12v, as does the rest. i'm lost.

my anode is a rod of graphite and cathode is ss

Posted (edited)

i could use a helping hand over here. my pc psu seems to be shutting off on me when i go and use the 5 volt side. as long as i'm not touching the electrode into the electrolyte the readings are fine. however when i do put in the electrodes the power is gone. now i can perform this same thing with the 3 volt side everything is just fine burpin away. whats this mean? also my fan doesn't seem to be working either. i'm pretty sure i've done the wiring right, all readings on my volt meter are perfect...12v reads 12v, as does the rest. i'm lost.

my anode is a rod of graphite and cathode is ss

 

 

Hi Kiss,

 

It's hard to tell from your description whether there's a problem with your power supply or the set up or proceedure. Do you have the ability to add a photo of your system? Maybe that would allow us to determine if something else may be causing your difficulties.

 

If your set up and proceedures are fine, I suspect the power supply. If it's the power supply, is it damaged or does it have features that are getting in the way? Is it operating fine and the system is drawing down the power? Have you tried letting it run and just see what happens (will it correct itself or is it just not going to work?)?

 

As you see, there are more questions than answers at this point. Can you give us more information? Maybe we can help you get to the bottom of this.

 

 

WSMcool2.gif

 

Another thought: have you considered posting the question in the electronics section? Maybe someone there can give good advice or instruction about computer supplies (since they vary widely depending on the intended application). Let us know what you find out.

Edited by WSM
Posted

hello WSM,

nice to meet ya.

welll i'd love to be able to take a photo for ya, but i dont have the means. i posted this problem of mine on another forum, and one of the replys had said there might be a sense wire? i've heard of this before. however not on the 5volt side. i was under the impression that is most commonly found on the 3volt side. the poster had told me to hook up a pc fan as the load before my cell. does this make sense? the fan thats built in hasn't turned on at all since i cut the wires and grouped them. this unit was tested at the store and was find. i'm lost.

heres another one for ya...... when i drop in my electrodes (5 volt side) plain water the unit seems to be working. if i do the very same thing but have a saturated solution of electrolyt the problem starts unless i use the 3volt side.

Posted

i hope you gys don't mind me asking...?

Would a graphite cathode perform better then a SS cathode?

I'm under the impression that SS undercertain conditions could cause iron oxide, which of course is not what i'm after. After roughly 18hrs. of operation I'm left with some black sludge with a bit of brown coloring to it. I can,t help but think that some of this might be iron oxide...could be wrong though.

Posted

i hope you gys don't mind me asking...?

Would a graphite cathode perform better then a SS cathode?

I'm under the impression that SS undercertain conditions could cause iron oxide, which of course is not what i'm after. After roughly 18hrs. of operation I'm left with some black sludge with a bit of brown coloring to it. I can,t help but think that some of this might be iron oxide...could be wrong though.

 

I use graphite anodes and cathodes and it all works fine.

 

Used to have a ss cathode, works well but breaks down if left in the solution without power.

Posted

i hope you gys don't mind me asking...?

Would a graphite cathode perform better then a SS cathode?

I'm under the impression that SS undercertain conditions could cause iron oxide, which of course is not what i'm after. After roughly 18hrs. of operation I'm left with some black sludge with a bit of brown coloring to it. I can,t help but think that some of this might be iron oxide...could be wrong though.

 

Becareful, there is a lot of quality of stainless steel. If you use a poor SS cathode it may not resist as well. But even for a poor quality SS, 18 hrs is really short. What is the distance between your electrode?

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