making potassium (per) chlorate

[taiwanluthiers]

One way to know for sure if you are wondering is add conc. sulfuric acid to the suspected perchlorate. If the purity is sufficient it will not react at all. If it is chlorate it will turn yellow and pop and crackle. Another way is wash it with icy water since perc is nearly insoluble in icy water but chlorate is still somewhat soluble in icy water.

[Thunder75007]

OK. The mystery is solved. I am not freaked out anymore, just saddened. I must flown past the KCL-> KCLO3->KCLO4 without stopping information, because it did not soak into my little pointed head. I just ran from KCL to KCLO4 without stopping. In theory, my anodes should be fried and they may be. The coating is not coming off of them but one is now yellow and the other is turning yellow in some locations. They are no longer the uniform grey that they were. The amperage on my second cell, after an 11 ½ day run, had dropped to 5.3 amps by this morning.

 

Before I filtered the second cell, I examined it carefully and it is evident where the KCLO3 stopped forming and the KCLO4 started forming. There is a very distinct line in the material in the bottom of the cell and the crystals on top of that line are not KCLO3. Apparently I have moved on to making KCLO4 without intending to. After I re-crystallize, I will see how much of the KCLO3 that was originally formed in this cell has changed over to KCLO4. Right now, it appears that the KCLO3 is by far the largest amount in the cell, judging by the distinct line. Oh well, now to buy some more cheapie Platinized anodes from EBay. They appear to work really well, if you don’t abuse them as I just did…..

 

The powder that I had referred to in the prior post is indeed KCLO4. I had just never seen it precipitate out of solution before, as I have not tried to make it yet. I thought that I could keep topping the cell off with a saturated KCL solution as needed and run this long. I was just trying to get to the weekend before clean-out. NOT!!! Lesson learned!

 

I still do not know what those little tiny hair/fiber crystals are, that precipitated out first. I will see if it happens on this run also. Whatever they are, they are less soluble than KCLO4 in water.

 

I only wish that I had found this forum months ago. It would have saved me a lot of time and grief. I have been gleaning information from all over and taking it with a grain of salt. As you all know, there is a lot of wrong and dangerous information on the internet. Here the information is accurate and the senior members keep you in-line! I very much appreciate this as I want to be as safe as is possible while perusing my interests. In this particular arena, I am a new-be. I must admit that I have never posted on other forums, even to ask questions. I just keep to my-self. But for some reason I decided to post on this one.

 

A wise man once told me, and I try my hardest to live by it, (Every man is my superior in that I may learn from him.) Even in areas where I am a qualified expert, I found that if I would get off of my high horse and listen to others ideas and information, I can learn even more.

 

I will post some pictures later of my above listed observations.

Edited August 9, 2014 by Thunder75007

[Thunder75007]

Thanks Taiwanluthiers. I have not done this as of yet but I suspect that I will get a reaction. I did see KCLO3 crystals forming at the end of the cool down run. As a guess-ta-mation, I would say between 5 to 10% is KCLO3. Therefore, the whole batch should be treated as KCLO3, according to what I have learned. I will try it though, just for grins. I may try the icy water wash as you suggested and then try it again if I do get a reaction.

Edited August 9, 2014 by Thunder75007

[pex]

Put it back in your cell and let it go for a few days extra. If the tempature drops. It's done. I think 2 or 3 days is enoug.

 

Pex

[Thunder75007]

Thanks Pex. I will try.

[WSM]

I just checked this thread and, Wow! When I get to Mason City, I'll try to catch up (I'm in a plane in Chicago right now).

WSM

Edited August 10, 2014 by WSM

[Thunder75007]

I have re-crystallized the second cell now and during cooling, I had the exact result as I have already described. There were more tiny hairs/fibers drop out in this one. When they collect on the bottom of the flask, they look like a white dust bunny.

 

I will attempt to attach some pictures now:

In this picture where you can see the line in the cell, where different crystals started forming.

This is a picture of my yellow tinted platinized anode.

This is how I connect the cells to run product.

This shows the different lawers of epoxy and or JB Weld covered by RTV Silicon.

This is the configuration of the first cell that I ran.

This is a shot through the side of the flask during cooling. The white stuff on the bottom is the fibers.

I tried to take a shot down the neck of the flask but the steam made it difficult.

 

All of this has caused me to take a step back and look at things. When I get into something I have a habit of going whole-hog! Giving this further consideration, I am not going to make a bucket cell. For the very small amounts of KCLO3 or KCLO4 that I would be using, I don’t even need to keep these cells running constantly.

I may try to increase the efficiency of these cells, because I like efficient!

Edited August 10, 2014 by Thunder75007

[pex]

Thats nice looking. I like the connection. Between the 2 cells. I gonna try this in the future with 2 big bucket cells. I thing 30 liters Each. Good Job

[Arthur]

Thunder

Are your cells wired in series or parallel?

[Thunder75007]

Arthur, they are running parallel. It does not matter which cell that I connect the power supply to.

[taiwanluthiers]

It's weird... I ran KClO3 and it just eroded the anode completely without producing any perchlorate. I wonder what happened.

[schroedinger]

Did you wanted to make kclo3? Then it sounds like you wired her up ir the wrong direction

[taiwanluthiers]

I wanted to make perchlorate. I didn't wire it wrong because if you wire it wrong it will not work at all (I tried). Ti is a valve metal so it will not work as anode at all.

[schroedinger]

Ok, then which type of anode you used?

Wiring it in the wrong direction just doesn't work if you use ti as kathode, with iron other ones it works and f0gives quite a mess, did that ones when i wanted to remove the mno2 coating from an anode. It got damaged as it was quite long used and i wanted to put a new one on. Bad idea now that anode serves as a kathode and i made a whole new anode up.

[taiwanluthiers]

anode was platinum. I just wasn't sure the chemistry going on, all I know was that I can smell ozone as soon as the cell runs, but it seems almost like nothing was happening in the cell apart from anode destruction. The chlorate seems to get recrystalized but not turned into perchlorate.

[pex]

That is realy strange. I used platinum platinized anodes. They dont holde long. But you can get a few kilo of perchlorate with out anny problem. I think three is realy someting wrong with your power supply. I used pbo2 and platinized with out anny problem.

[taiwanluthiers]

What do you think could be wrong? I only notice the current draw was very low, like 5 amps at the very most with a fairly concentrated hot pot. chlorate solution. It actually starts out at like 8 amps or so but as the solution cools (it couldn't get hot enough on its own to maintain it) the current draw just goes down, and nothing seems to form apart from pieces of anode falling off.

[pex]

Try sodium

It's better for your anode. A tip from my try a glass aquarium heater. Than your Temperature stays arround 40 ddegrees. I tried this and it Works realy good.

[MrB]

That is realy strange. I used platinum platinized anodes. They dont holde long. But you can get a few kilo of perchlorate with out anny problem. I think three is realy someting wrong with your power supply. I used pbo2 and platinized with out anny problem.

With the price of platinum anodes what it is, it turns out to some freaking expensive perchlorate... Of course, this depends somewhat on the size anode needed.

I'm also somewhat confused. eBay is cheap for anodes, claiming to be platinized titanium mesh anodes. There is hardly any plate anodes at all. Now, my question would be...

Is there a significant advantage to plate over mesh, or the other way around? I'm thinking plate gives a lot more surface area, and uses significantly more titanium & platinum, while the price increase isn't actually that significant. (That is, the increase between mesh, and plate. Now, the price increase just to start looking outside eBay, seams a lot nastier...)

 

I haven't got a clue still. This whole thing freaks me out, i want my pyro to be reliable, and preferably cheap.

B!

[schroedinger]

Yes, plating on a plate tends to give a layer with internal stress in the coating, which make it prone to crack quite easy. The mesh anode is helping in reducing these.

[MrB]

So mesh, even tho being a LOT less surface area is a better alternative then plates. Ok, thank you for explaining how / why. Only way i'll ever figure this out, i'm afraid. Having someone explain it to me, very slowly. And as if i was a freaking moron.

B!

[schroedinger]

No worries about that, I'm pretty sure everyone here knows that you are really interested in learning all these things and won't bugger about explaning.

 

Also a mesh anode ist that lot smaler then a plate one. Specially not a ld anode, as it fills up nearly all holes.

[pex]

Try to gett a pbo2 anode. I think this is the cheapest and most easy way to make perchlorate. I never had anny problem. Even with a damaged anode i succest to make 15 kilo perch.

[pex]

Try to contact chinese factories. They will some times shipping for a few anodes. And they have good prices to

[pyroChile]

I have re-crystallized the second cell now and during cooling, I had the exact result as I have already described. There were more tiny hairs/fibers drop out in this one. When they collect on the bottom of the flask, they look like a white dust bunny.

 

I will attempt to attach some pictures now:

P8090031.JPG In this picture where you can see the line in the cell, where different crystals started forming.

P8090035.JPG This is a picture of my yellow tinted platinized anode.

P8090037.JPG This is how I connect the cells to run product.

P8090040.JPG This shows the different lawers of epoxy and or JB Weld covered by RTV Silicon.

P8090045.JPG This is the configuration of the first cell that I ran.

P8090048.JPG This is a shot through the side of the flask during cooling. The white stuff on the bottom is the fibers.

P8090050.JPG I tried to take a shot down the neck of the flask but the steam made it difficult.

 

All of this has caused me to take a step back and look at things. When I get into something I have a habit of going whole-hog! Giving this further consideration, I am not going to make a bucket cell. For the very small amounts of KCLO3 or KCLO4 that I would be using, I don’t even need to keep these cells running constantly.

I may try to increase the efficiency of these cells, because I like efficient!

 

Hello Thunder!

 

Where did you buy these anodes? some link?

 

I bought it, but at a price of $ 125...

 

 

best,

 

 

=)