making potassium (per) chlorate

[WSM]

Here it's my solution for poor's man HCl dosage system A dilute solution of HCl (0.5M) is in the bottle.

 

http://img9.imageshack.us/img9/9387/picture023ti.th.jpg

 

http://img89.imageshack.us/img89/2936/picture022he.th.jpg

 

Hey 50AE, if it works for you, great! I think any method that achieves the desired results, safely, is a good method.

 

I'm trying to take the lazy way out (which, unfortunately, is more expensive). I'm still deciding whether to use Swede's gravity fed system or just adapt elements of it in a different variation. Either way, using pH control is much more efficient and, therefore desireable.

 

Congratulations on taking the next step in efficient and effective chlorate making .

 

WSM

[50AE]

Hey guys, I found a very cheap MMO mesh supplier. Has anyone had experience with this seller? Or another eBay seller?

 

http://cgi.ebay.com/EXPANDED-TITANIUM-MESH-STRETCHED-SCREEN-MMO-COATING-/260747402496?pt=LH_DefaultDomain_0&hash=item3cb5c19d00

[bikemaster]

Hey guys, I found a very cheap MMO mesh supplier. Has anyone had experience with this seller? Or another eBay seller?

 

http://cgi.ebay.com/...=item3cb5c19d00

 

This guy sell cheap MMo mesh for over a year. I buy some from him about 10 month ago and it was all good. You will maybe need to wash the anode before to use them, because some of the have a brown deposite on them. Just let them in a HCl bath for 15-20 min and they are clean.

[WSM]

Hey guys, I found a very cheap MMO mesh supplier. Has anyone had experience with this seller? Or another eBay seller?

 

http://cgi.ebay.com/...=item3cb5c19d00

 

Hi 50AE,

 

Yes, laserred is an excellent supplier.

 

Swede bought a lot of the material he was selling from him. I've also purcahsed this material (first from Swede and then direct from laserred). It has a thicker titanium substrate and has a thicker MMO coating than many other suppliers use. Sometimes the material has a brown coating on it which Swede recommended removing by soaking in HCl for 15 minutes. The HCl cleans off the brown smut without damaging the MMO or titanium.

 

The MMO offered does not have a lead and one needs to be applied to make the best use of it as an anode. I believe the best type to use is a tubular lead, made the way Swede shows in his excellent blog. Tubular leads can be sealed in Kynar compression fittings in the lid of a cell, preventing the annoying salt creep that can damage the electrical connections to the electrodes. Swede recommended removing some of the MMO coating before spot welding (or TIG welding) leads on, but in an experiment, I discovered that I could get a good spot weld to this MMO/Ti material without first removing the coating; by using heavy pressure and running the spot welder longer than with lighter guage titanium. I ran the spot welder till it "complained" (growled loudly, and I could just begin to see glowing metal around the point of contact). I stopped at that point and saw I had a good weld point. I repeated the process till I had a good pattern, like shown in Swede's blogs.

 

Laserred is a good supplier and has very low rates. I recommend his material and excellent service (fast shipping). I believe he offers international shipping as well. I am not connected with laserred in any way, other than as a satisfied customer .

 

WSM

[50AE]

Much thanks guys! I'm going to buy in bulk from him.

Can you help me with the finding of cheap supplier of CP grade titanium? Rod or sheet, it doesn't matter.

[WSM]

Much thanks guys! I'm going to buy in bulk from him.

Can you help me with the finding of cheap supplier of CP grade titanium? Rod or sheet, it doesn't matter.

 

Try looking for CP titanium on eBay. There is a supplier of surplus titanium in Latvia who has several listings.

 

WSM

[athlon]

I had forgot about a batch of NaCl that I wanted to test to convert to KClO4 in the end and now I have gotten a precipitate at the bottom of the jar that's rock hard and I'm not able to break it up without destroying the jar.

 

Is the precipitate NaClO3? I'm just so confused as KClO3 didn't get like this.

If so then I just need to dissolve it and continue the electrolysis with a platinum anode I guess.

 

Edited March 12, 2011 by athlon

[WSM]

I had forgot about a batch of NaCl that I wanted to test to convert to KClO4 in the end and now I have gotten a precipitate at the bottom of the jar that's rock hard and I'm not able to break it up without destroying the jar.

 

Is the precipitate NaClO3? I'm just so confused as KClO3 didn't get like this.

If so then I just need to dissolve it and continue the electrolysis with a platinum anode I guess.

 

Hi athlon,

 

If it started as NaCl and you're using an MMO anode, I suspect either NaClO₃ or a mixture of NaCl and NaClO₃.

 

Quick Test:

If you can get a sample, grind it to powder and mix it with a little charcoal powder or powdered sugar and burn some (in a safe place) and see if it reacts like chlorate or not. An alternetive test would be to sprinkle a little on a glowing piece of charcoal in a barbeque and look for a reaction when the salt hits the charcoal.

 

These tests are rough and not as definitive as using chemical analysis, but a quick way to determine what you have. If you decide there's chlorate there, you can rehydrate it, add NaCl and continue to run it to get more chlorate for feed stock for a perchlorate cell. If you feel it is primarily chlorate (low chloride), then go ahead and rehydrate it and run it in the perchlorate cell.

 

What fun! Let us know what you find.

 

WSM

 

PS - Next time, label the container to keep track of what's inside (don't worry, I think we've all done this before).

Good judgement is born of experience. Unfortunately, much experience is born of bad judgement .

[50AE]

Keep in mind that NaClO3 is more than 2x more soluble than NaCl at 0C, and solubility increases in a non linear way, it gets 5* times more soluble at 100C.

[pdfbq]

I made kilo's of KClO4 the NaCl -> NaClO3 -> NaClO4 ->KClO4 way.

To me it looks (and 'feels') much like NaClO3

[WSM]

I made kilo's of KClO4 the NaCl -> NaClO3 -> NaClO4 ->KClO4 way.

To me it looks (and 'feels') much like NaClO3

 

Though I like the idea of avoiding sodium contamination in oxidizers planned for color compositions, the problems of solubilities of the potassium salts has me rethinking the perchlorate process.

 

I still will go directly from KCl to KClO₃ for potassium chlorate. But, for perchlorate production, I'm starting to lean toward starting with NaCl and go to NaClO₃ using MMO and titanium; and then switch to LD and titanium for the NaClO₃ to NaClO₄ process and afterward exchanging NaClO₄ with KCl to produce the KClO₄ end product.

 

After a few washings with chilled distilled water the potassium perchlorate should be very pure (no sodium contamination).

 

Nothing is set in stone, but these are the thoughts I'm having.

 

WSM

[pdfbq]

There are some advantages using the NaClO4 way I think.

You can have a MASSIVE amount of NaClO4 in 1 liter of water, so a small cell will do (I used a 2 liter cell and it produced 1.25 kilo's of clean KClO4 in five days.

No salts jamming your cell half way

Chlorate destruction is very easy because of the solubility. Just add 50 grams of sodium meta bi-sulfite, heat slowly and you're done.

You can make other things from NaClO4, NH4ClO4 for instance.

 

Getting rid of the NaCl is a bit of work. Two times recrystallization will definitely do it, but a KClO4 cell also needs recrystallization I guess.

Edited April 6, 2011 by pdfbq

[Bonny]

There are some advantages using the NaClO4 way I think.

You can have a MASSIVE amount of NaClO4 in 1 liter of water, so a small cell will do (I used a 2 liter cell and it produced 1.25 kilo's of clean KClO4 in five days.

No salts jamming your cell half way

Getting rid of the NaCl is a bit of work. Two times recrystallization will definitely do it, but a KClO4 cell also needs recrystallization I guess.

 

How many amps were you driving into the cell? It's been awhile since I ran a cell so I don't remember the a/h needed...

 

I never had any issues with salt build up on my perc KClO3 --> KClO4 cell. I was using Pt anodes (that I fried).

 

My perc was recrystallized to remove chlorate. I only tried chemical purification (using potassium meta-bisulfite) once and ended up with a mess - there's an earlier post IIRC.

I think 2 recrystallizations + washings with cold water/alcohol will remove the chlorate, as even after a single recrystallization, chlorate was almost undetectable using NPAA.

[pdfbq]

Amps were I believ 18 -> 14 ( you need much less to produce perchlorate from chlorate than chlorate from NaCl )

I did not fry my Pt anode, its stil alive, but not 100% anymore for sure.

 

Chemical purification is I believ more easy with NaClO4 because your liquid is so concentrated. You just need a little bit of the meta bi-sulfite to bubble all your solution.

Its I guess the only way if you want to make not only KClO4

[WSM]

Amps were I believ 18 -> 14 ( you need much less to produce perchlorate from chlorate than chlorate from NaCl )

I did not fry my Pt anode, its stil alive, but not 100% anymore for sure.

 

Chemical purification is I believ more easy with NaClO4 because your liquid is so concentrated. You just need a little bit of the meta bi-sulfite to bubble all your solution.

Its I guess the only way if you want to make not only KClO4

 

Hi pdfbq,

 

Thanks for the info, but I'm wondering how my Chinese LD anode will hold up? Anyone try one of patsroom's LD anodes yet? I will do mine later but am "all ears" about other's experiences before I get around to it .

 

WSM

[Bonny]

Anyone try one of patsroom's LD anodes yet? I will do mine later but am "all ears" about other's experiences before I get around to it .

 

WSM

 

I've got one... but you got yours first!! I'm waiting for you to do some testing. I have enough perc for awhile, so I haven't needed to try mine.

[WSM]

I've got one... but you got yours first!! I'm waiting for you to do some testing. I have enough perc for awhile, so I haven't needed to try mine.

 

Hi Bonny,

 

Thanks for the feedback. My whole world is on hold while we are getting ready for my Daughter's wedding at the end of the month. Also I have several tool orders to fill before I can work on electrochemistry with a clear conscience.

 

I hope your LD anode came in better shape than mine. Somewhere between patsroom's place and mine, the post office did a number on the box and a little damage occured. I'm going to try to repair it but I'm afraid the active cell may cause a separation between the base metal and the LD plating . If that happens, it's all over for the electrode . I haven't heard from patsroom so I don't know if he's still in the LD electrode business any more.

 

If you get started using yours before I can with mine, let me know how it works. Thanks.

 

WSM

Edited April 9, 2011 by WSM

[50AE]

I got a MOT ! It was a little difficult to remove the 2nd winding from it, but I managed. Gonna build my new cell power supply soon!

[WSM]

I got a MOT ! It was a little difficult to remove the 2nd winding from it, but I managed. Gonna build my new cell power supply soon!

 

I don't understand, what is a MOT? Can you please explain? Thanks.

 

WSM

[50AE]

It means microwave oven transformer.

[WSM]

It means microwave oven transformer.

 

Hi 50AE,

 

Wow, it sounds like an ambitious project. Good luck with it ! I've been fortunate to have access to occasional good deals on workable power supplies. My first one, though, was cobbled together from a collection of transformers and a full wave bridge rectifier. It worked but wasn't terribly efficient .

 

WSM

[pyrojig]

What are you wiring the MOT to run at? Amps/volts? If Im not mistaken, these can handle very high Amperage , and be whatever voltage you wind it to be. I think in the range of 50+ A ..

What size cell(s) are you running with this supply ?

Where did you score your power supply from ( old micro, junk , or purchased new for the use of a MOT) ?

AM I correct in guessing that the older micro's had a massive powersupply compared to the newer ones?

[WSM]

I got a MOT ! It was a little difficult to remove the 2nd winding from it, but I managed. Gonna build my new cell power supply soon!

 

Can you post photos?

 

WSM

[Arthur]

Microwave oven transformers are about a 750watt chassis. There is a mains winding and one at several KV -be careful!

They are best used for short duty cycle applications and "spot welder" is probably the best second use for a MOT. For an electro chemical cell cut off the HV winding and wind a few turns of thick wire (insulated) and see what current /voltage that you get add or subtract a few turns. MOTs are nice because they use few turns per volt so you don't have to wind many turns of thick wire to make a product. However this makes the transformer inefficient in continuous duty applications.

[50AE]

The main problem because I won't use it is its consumption - 3,6A at 230V = 830W ! If I run this thing for about a month, it's gonna eat my wallet for electricity bill. It would be useful if I could make a cell with 100A current pumping into it, but I really can't do that. So I'll look for another option.