making potassium (per) chlorate

[WarezWally]

I cover all my connections with hot glue and directly solder my wires to the connections on my graphite anodes. Before this I had a alligator clip disappear in the space of a week

[jacob]

Wally, this guy says he has had success with Lead dioxide/epoxy anodes.

[WarezWally]

I wouldn't trust that ebay guide

 

Recommends copper cathodes

Uses ultra low purity lye for pH adjustments

No real measurements (how big is a few cap fulls?)

No mention about ammonium chlorate when making ammonium perchlorate, just tells them to destroy chlorate while talking about sulfur.

Thermal decomposition of kclo3 to kclo4

[WarezWally]

I may have found a commercial source for lead dioxide anodes, a ebay seller who sells MMO and pt plated anodes thinks he may be able to get lead dioxide anodes from his supplier. Hes looking into it for me, if they are cheap enough I think i may have solved my perchlorate problem once and for all.

[BPinthemorning]

I had my first yeald of potassium chlorate last night! I'm purifying it now, and I'm gonna try it out.

[BPinthemorning]

I have about 50 grams yeald. Should i just throw the laquer back into the cell, or do I ad more chloride?

[tentacles]

If you're just making chlorate, when you top off the water use a saturated chloride solution. Before you recycle that liquor, you could try and dissolve more chloride in it - it wouldn't hurt anything to resaturate the solution.

 

I picked up a couple pounds of lithium carbonate while I was on vacation at a nice $6.45/lb. Going to convert to chloride.

 

Mumbles: can I convert the lithium carbonate to chloride by reacting with a calcium chloride solution? I'm not certain what the reactivity for metal salts is - what ion would replace another preferentially. Is there a chart for this, somewhere? I know that lithium carbonate is just barely soluble (and less so as the water heats up).

[Bonny]

I'm not certain what the reactivity for metal salts is - what ion would replace another preferentially. Is there a chart for this, somewhere? I know that lithium carbonate is just barely soluble (and less so as the water heats up).

Tentacles, I think I have an (old) table at home that list metals in order of displacement characteristics. I'll check when I get home and email you the info.

[BPinthemorning]

i have a displacement chart, i just dont know how to get it on...

[Mumbles]

The thing you think you're looking for is the "Activity series".

 

http://www.unr.edu/sb204/geology/mas.html

 

However, it has nothing to do with what we're talking about here.

 

It should work theoretically, if you can get enough into solution. The chart you want to look for here is the Ksp chart. The most insoluble product will be favored.

 

I think the best plan of action however is HCl. It will neutralize the carbonate into CO2, and LiCl.

[BPinthemorning]

thats the one my chem teacher gave me. I hate my chem class. I'm in an honors class at a privat school, and the semester is over in 3 weeks, and we have done a grand total of 3 labs... I do more chemistry at home then I do in my chemistry class... Nothing but notes and worksheets.

[WarezWally]

My local fert supplier doesn't have any KCl in stock and I'm told it will take a month to arrive if I order some more in. This doesn't leave many options, I have a found a place that sells KCl as a horse supplement. Would it be reasonable to assume that it would be ammonium salt free?

 

http://www.valueplus.net.au/cat/?op=sp&id=189

 

They also sell cheap sulfur which according to the MSDS is 100%

 

 

/Ive emailed for a MSDS but I am not counting on getting ones.

 

Cheers

[Bonny]

I think the best plan of action however is HCl. It will neutralize the carbonate into CO2, and LiCl.

I'm assuming this would be similar to making CUCl2 or SrCl2 using the carbonates and HCl?

 

Also, I posted the info I have on elements in electrochemical series here: http://www.apcforum.net/forums/index.php?s...=20entry25936

 

Probably no good for what Tentacles is doing but might be handy for some other things.

[Mumbles]

Yep, pretty much exactly the same. The same reaction holds true for most carbonates. I am unsure about lead and silver carbonates though, but really you'd have no use for these chlorides.

[tentacles]

silver chloride is useful as an intermediary in purifying sterling silver (only slightly off topic). I used the method on the chlorates website to purify sterling that I used to plate silver on my anode.

 

The cell's still running. I picked up a +-50A current meter (automotive type) to monitor the cell's current in a broad sort of way. I filtered off all the brown PbO2 dust last night, no real reason but the liquor is very clear. A bit on a popsicle stick burns bright yellow, definitely some oxidizer in there. Have not tried to cool the liquor or test for perchlorate yet.

 

I picked up some methylene blue at a pet shop recently. Can anyone describe the process for testing for perchlorates? The information I've found is pretty general. Does the solution stay blue if there is no perch, or does it turn clear?

 

The anode seems to be holding up fairly well. The spotty growth areas on the sides are eroding a bit, but the smooth areas are pretty solid. No signs of copper eroding in the solution, it was very clear and I put more lacquer over the connections.

[tentacles]

Wanted to post an update. The anode failed today, due to the chewy hollow center (where the NC + PbO2 powder used to be) wicking up electrolyte to the electrical connection. I'm actually pretty impressed by how long the connection lasted, considering that it's probably been soaking for two weeks. The anode has eroded some, but the smooth areas in the center don't seem to have eroded at all.

 

I have a strip of filter paper drying with some of the electrolyte on it. The liquid is almost syrupy. Going to spark that up later to see if there's any oxidizing action going on.

[jacob]

There's a guy who sells pt anodes on ebay for a good price, he made some videos on youtube showing just how to make chlorates/perchlorates, they can be found here. worth a look.

[tentacles]

I actually have a Pt plated Ti anode, but I'd rather go with LD. It's kind of a moot point right now for me, but it's something pyro to do during the winter.

 

I boiled the liquor last night, it went from slightly yellowish to clear. It's about 1.5L now and upon cooling to 25C, I've got probably 75g of precipitated crystals. I picked up some potassium chloride today to convert with. The methylene blue turned purple in a test, but I didn't get any precipitate? The filter paper I soaked burned like fuse and alternately burned (quickly!) with a bright yellow flame. I've got at least chlorate, the purple indicates I probably have some perc.

[jacob]

I've had a cell running for about nine hours and one thing i've learned is Chlorine gas is BAD stuff, i had to replace the metal lid on the jar i'm useing becase it was breaking down and contaminating my solution.

[WarezWally]

There's a guy who sells pt anodes on ebay for a good price, he made some videos on youtube showing just how to make chlorates/perchlorates, they can be found here. worth a look.

Those vidoes are shit to be honest, I doubt he even made much (if any) perchlorate seeing as he was starting from potassium chloride. His end product was pretty much all potassium chlorate with a small amount of perchlorate.

 

He filtered his electrolyte at like 60c, he should read a solubility graph as he is loosing a lot of product.

[tentacles]

Finally got my Ti sheet yesterday, converted some lead nitrate into lead oxide, about 107g of that total. I "recharged" my plating bath from before; I put some Pb in and used a Ti anode and Cu cathode to plate out almost all of the Cu that had dissolved when the Pb ions plated out. It would have displaced the copper without the plating, but it went faster, even much more than I expected this way.

 

I should be able to plate out a good 200g of PbO2 from this new bath without the plating getting crazed like it did at the end of the last one.

 

I'm in need of some sodium fluoride for the next cell run. There's a place I can order from here in Canada, but I hate to wait for them to order it for me, and then ship it. I know persulfate is supposed to work, but the tests I've seen show the fluoride increasing cell efficiency more. Does anyone know if potassium fluoride would work as well? There'd be less risk of Na contamination with it. I may also be able to get calcium fluoride locally. Last time I was at the local ceramics shop the guy told me "we don't sell fluorides" when I asked for sodium fluoride. Sounded funky to me. I'll try calling them tomorrow maybe.

[WarezWally]

Compounds of fluorine

 

I though you couldn't plate pure Ti due to Ti oxide forming with is non conductive, you have to coat it with something first.

[Mumbles]

Calcium Fluoride (Fluorspar at the ceramic shop) is insoluble in water, so no go there. Potassium fluoride should work just fine though. It'd be converted to sodium very quickly anyway from the chlorate forming. It would precipitate potassium chlorate, and form sodium fluoride.

[tentacles]

Mumbles: would it be possible to convert the CaF to HF and react with NaOH/KCO3/etc using sulfuric acid? This could be relatively inexpensive and provide me with the instant gratification that I require.

 

Wally: my sheet isn't pure Ti, but the natural Ti oxides that form are electrically conductive. I'm not plating over the Ti; rather I'm trying hashashan's method of plating next to the Ti, into a scotch brite pad. I think mine is 6-2-2-2 alloy or something. It was loud as fuck to cut on my bandsaw.

 

On a completely unrelated note, there's been some really interesting discussion on science madness about the spinel cobalt platings as anodes. There's some promising stuff so far, but it looks about a bitch to plate on. The most promising ones use a pyrolisis technique rather than electroplating.

[jacob]

Those vidoes are shit to be honest, I doubt he even made much (if any) perchlorate seeing as he was starting from potassium chloride. His end product was pretty much all potassium chlorate with a small amount of perchlorate.

I found out later those videos weren't made by him, but a previous ebay anode seller. on another note, i've made about a pound of damp (Potassium) Chlorate and want to convert it to Perchlorate through thermal decomposition, my questions are, will this get rid of all the Hypochlorite? is this a good (as in complete) method of converting it? and what are the safety concerns?