making potassium (per) chlorate

[WarezWally]

Google just found me a holy grail, a photographic supplier who sells stuff for developing photos.

 

Among many thing i purchased:

 

500ml conc nitric acid

100g lead nitrate

 

anode here I come smile.gif

[BPinthemorning]

If you have the suplies to make an extra one, I would be glad to buy it off your hands if the price is fair. And Wally, what is the website you found?

[BPinthemorning]

I have run my cell for 5 days now, and I filtered all of the graphite off the solution. How do I extract my chlorate from my solution?

[WarezWally]

Damn, they wont ship the acids and I wont be in the area for at least a few months.

 

Is the nitric acid used to lower the ph vital?

[jacob]

How do I extract my chlorate from my solution?

Cool it down to just above freezing, and crystals should form that can be filtered off (i think), let me know what yield you get, i want to try this, but i don't have much use for Chlorates.

[tentacles]

Start by cooling it to freezing, and see if any precipitates out. How much g/l did you start with?

 

Sodium chlorate is quite soluble in water, so you may have to boil it down some to get chlorate to precipitate out.

 

read more here: http://www.geocities.com/CapeCanaveral/Cam...ate/remove.html

 

Wally: I could have sworn I posted a reply for you here earlier: you don't need the nitric, once you start plating out lead ion, the nitrate ion will form nitric acid with the water. What you will want is a supply of lead oxide to top off your solution with lead ions. I can definitely say you're going to want a whole lot more than 100g of lead nitrate; I used about 350g of it in 800ml of water, and I wish I'd had more to add. The lead oxide will buffer the solution and help, but with only 100g of lead nitrate, your solution would have to be less than 500ml, and you *must* have some lead ion to add to replace what is plated out (as it is plated out). You can't let the lead concentration fall below 200g/l.

 

Also, the more you plate out the more acidic the solution gets (this should be obvious). My copper cathodes dissolved at the end of plating - that's how acidic it got. Now my plating bath is full of copper nitrate. I can plate out or replace the Cu with lead ions). It's as simple as adding lead metal to the bath, the copper metal will fall out of solution. I'm going to try and get some pure Pb at work tommorow (I work at a scrap yard).

[WarezWally]

You did, just not here

 

http://www.pyrosociety.org.uk/forum/index....330entry40550

 

Damn green hippies have pretty much stopped the use of lead oxide in pottery, I could attempt to make my own but heating lead and blowing air across it for a few hours isnt exactly fun

 

Ive got shitloads pure lead to spare

[hashashan]

simpler :

 

Pb(NO3)2 + 2NaOH = Pb(OH)2 + 2NaNO3

 

Pb(OH)2 + heat(not much heat needed, a simple gas stove will do the trick) = PbO + H2O

[ibah]

Homemade perchlorate setup and results. Using platinum and stainless steel on 1 cell. Using platinum and titanium on the other. Hopefully link works. Flash makes a big whomp when lit, cant hear on video though

 

http://s231.photobucket.com/albums/ee182/ibah68

[WarezWally]

Looks good

 

What type of platinum are you using (plated, wire, ignot etc)?

[ibah]

One of them is 5" and is flat 1/4" i believe the plating is 2.5 micron. The other is 1/4" round stock by 6". I have tried the carbon or graphite type before but is a pain, it is messy and too many steps involved to aquire product, but can be done. If you can get platnium it is worth the money as they say.

[tentacles]

In that "1 day" pic - is that a recycled liquor, or are you doing chlorate -> perchlorate? I've been running mine a few days now (starting with nearly saturated NaCl) and don't have any precipitant - but considering the solubility of Na chlorate/perchlorate, I don't expect to see any crystals until I freeze it, or boil it down. Or are you using KCl?

[ibah]

Yes that is recycled electrolyte, every once in awhile I do boil it done and scrap the precitant and pour the soulution only in to the cell and run for about 2 days and repeat. Using potassium chloride 99.975% pure, as soulution. Yes I m producing chlorate then perchchlorate. If you are using a new setup run for 5 days straight then cool and repeat. When running you will barely see any crystals until the cooling process. If you are running cell and seeing fluffy precipitant and not crystals it ain t going to work, found that out hard way. Also running my cell in garage with no heat and I wrap the cells in fiberglass to keep the heat in, find running a little hot but when running produces little precipitant but when cools produces a fair amount more than usual precipitant. Also if you notice running 1 cell with platinum and stainless the soulution is more apple juice color. Running the other with platinum and titanium the solution is clear. Also another note if using stainless steel take out during cooling or it contaminates the solution, turning the solution darker, another lesson learned hard way

[jacob]

I thought that going straight from Potassium chloride to Potassium perchorate was hard to do because Potassium chlorate is mostly insoluble, and it tears up your anode. am i missing something here?

[BPinthemorning]

What should I do to keep the chloride levles up in my cell? Also, what kind of local store can I get carbon gouging rods from?

[jacob]

Um, add more chloride? and welding shops shlould have those rods, although they may be copper coated.

[ibah]

Not sure what you mean Jacob. But I precipitate from the second day and what is precipitated is potassium chlorate, I then bake the chlorate when it is dry, in about two days, then bake to get potassium perchlorate. Then I take the saturated liquid, once crystals are scooped out and put back into cell to get more chlorate, then dry and bake crystals to get perchlorate and so forth. Carbon rods at any welding store. As for getting chlorine levels up just let cell run a few days more and keep adding soulution once evaporated.

[jacob]

Oh ok, i understand now, for some reason i thought you were going straight from Potassium chloride, to Potassium chlorate, to Potassium perchlorate all in the same run, which i didn't think would work.

[hashashan]

ibah : you use thermal decomposition of chlorate to get perchlorate???? hell ur a brave person

[WarezWally]

Looking to replace my SS cathode with titanium, I have a sheet of 6A4V but:

 

1. Its a bitch to cut

2. Not that great

 

I have a few otions on what to buy:

 

http://cgi.ebay.com.au/Medical-Grade-Titan...1QQcmdZViewItem

http://cgi.ebay.com.au/Titanium-tube-tube-...1QQcmdZViewItem

http://cgi.ebay.com.au/Titanium-tube-tubes...1QQcmdZViewItem

[hashashan]

Ti is not such a bitch to cut. i cut about 15 cm of 3-4mm plate in less then 10 minnutes

[WarezWally]

Tell that to my hacksaw

[Mumbles]

You may want to consider getting a higher quality blade in that case. My tool knowledge is mediocre at best, but cutting titanium isn't all that unheard of nor suspicious if you ask an employee.

[Bonny]

Tell that to my hacksaw

As Mumbles said a better quality blade should help. Cutting slowly with good pressure should prevent the material from heating up and "work hardening" Oiling the blade while cutting is another thing to try. Cutting oil would be best (hardware store) but any oil is (usually)better than none.

[tentacles]

Just about the only good use for WD40 is as a cheap cutting fluid - it works reasonably well for this. As Bonny said, the biggest problem is the work hardening of some alloys. CP titanium is quite soft and should cut easily. Ti is certainly no more difficult to cut with a saw than a hard steel, and easier to cut than stainless. Try a "bi-metal" blade. Or go by a local welding shop and have them cut it on their ironworker machine/cutting brake.

 

I tweaked my cell some yesterday, I had originally attached the Ti wires to a copper wire by simply twisting the two together - this worked well enough at first, but as the ClO2 gas oxidized the copper, the resistance was going up. I was losing about .5v at the connection so I thought of screwing the wires to a copper strip. Not having a copper strip, I cut a 1.25" strip of 1/64" PCB and bent it into a hoop, and soldered a 10 gauge copper wire to hold it in a circle shape. I screwed the wires to the copper strip with nuts and screws, and the loss is only .05v per wire now, much better. I have some precipitated silver drying that I will attempt to use as a paste/interface to lower the connection resistance further. The PCB should be able to handle ~60A without heating up much.