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Making (Per)chlorate electrodes


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Posted

hello everyone,

 

since nobody else bothered to make this topic, i went ahead and made it so we can all stop discussing making and generally discussing about electrodes, more specifically anodes, which are best to use in (per)chlorate cells.

 

mumbles, do you mind cutting pages 52-current from the "making (per)chlorate " topic, as it really should belong in here, as you said..........

 

 

 

 

anyway, i just bought a large 10"x6" MMO anode and i need to learn how to use it. first ill come up and ask this.

who here has experience with electrically conductive glue in a chlorate cell?

i dont think i can use a welder (spot welder works apparently, but not a welder) to weld some titanium sheet onto my anodes, so at the moment im considering using electro conductive glue, which i just orderd from ebay. does anybody here know what may happen to it in a chlorate cell , out of the water?

Posted
I've been busy with stuff lately. I was going to and still will get to the movement of the posts. Patience is a virtue. They're going to show up before your initial post, but I'll make it work out.
Posted

nono, thats fine, i dont mind having to delete my first post if it makes more sense to the forum topic. but if you don't mind shifting it that'd be great

 

 

what i want to say now though is that i have bad news. i did a bit of research into lead acetate for lead dioxide electrode, and unfortunately, it makes lead dioxide alpha! though it can still be plated on rather densely if other additives are included like soap or potassium hydroxide to the electrolisis bath.

 

im still going to attempt to make an electrode and i ill try to make perchlorate from it. i am also going to go and try and get a large quantity of lead nitrate, and make lead dioxide electrodes to sell on my site, as it has already been confirmed it will form beta.i might go to a wholesaler (alibaba) once i get some money to invest!

something i wish to ask here though is, will i be able to salvage the nitric acid from the lead nitrate bath?

ive done some reading, and people have put other lead compounds like yellow lead and lead carbonate into the lead plating baths to add more lead to the anode, which got me thinking, "doesn't this mean that the acid is reacting with this lead?".

hence the presence of acid, or are the nitrate ions floating in the water making this reaction?

 

because if i can, i might spend some time making sulfuric acid(from copper sulfate) to make nitric acid from potassium nitrate, which i can use over and over again to make lead dioxide anodes!

Posted

The problem you're going to run into is that you need to keep the pH controlled in order to properly deposit the electrodes. Thus any nitric acid formed is going to need to be neutralized every so often. This is where the lead carbonate or oxide come into play. It has more than one purpose. Trying to get the "spent" liquid back down in pH with commonly available acids to harvest nitric acid is going to introduce ions that will immediately precipitate lead (sulfate or chloride).

 

Have you actually done research on how to properly plate lead dioxide electrodes? You seem to overlooking a lot of key things. If you actually want to be able to sell these, you may want to drop the clandestine methods. Get real chemicals of known purity and composition, and use them to make the electrodes.

Posted
yes, i have done research, but i always like to have a second opinion on most things before i can tell myself its a fact or this is what it is
Posted

yes, i have done research, but i always like to have a second opinion on most things before i can tell myself its a fact or this is what it is

 

Hi OMBJ,

 

Somewhere in Swede's blogs is an entry on making an LD anode, and how he (finally) managed it. There are a lot of details and even though the final success wasn't perfect, it was very encouraging. Using Swede's method plus learning from it to avoid the pitfalls should lead to ultimate success.

 

For what it's worth...

 

WSM B)

  • 2 weeks later...
Posted

At the moment i have a theory.

 

when a lead nitrate lead dioxide plating cell is running, it generates nitric acid and lead dioxide. if there is too much nitric acid however, it will prevent the lead dioxide from being plated on the anode, as the current is obviously too slow to plate more than the acid is eating away.

what i want to do, is rather than boil off the acid, i want to neutralize it with lead and copper oxides which will obviously increase the ph and lower acid levels and provide more lead for the cell.

 

would this work while its running, or will i need to turn it off first?

Posted

At the moment i have a theory.

 

when a lead nitrate lead dioxide plating cell is running, it generates nitric acid and lead dioxide. if there is too much nitric acid however, it will prevent the lead dioxide from being plated on the anode, as the current is obviously too slow to plate more than the acid is eating away.

what i want to do, is rather than boil off the acid, i want to neutralize it with lead and copper oxides which will obviously increase the ph and lower acid levels and provide more lead for the cell.

 

would this work while its running, or will i need to turn it off first?

 

I think Swede added lead monoxide (but not more copper) so the lead levels would stay high enough to keep plating, even though the lead is being used in the process. Swede mentions the Patents he gleaned the info from and which ones worked the best for him. See if his writting in the blog helps...

 

WSM B)

Posted
well copper is rather reactive with nitric acid, im certain any copper forming would go back into solution keeping copper levels constantly high enough to keep lead flowing to the anode.
Posted
You'll certainly be able to tell if the copper is reacting if during the electrolysis NOx is given off.
Posted

damn.... thatle mean that ill be loosing nitric acid...... but surely the there wouldnt be so much copper forming at the cathode that it would start bubbling off NOx, after all, im pretty sure swede was even using copper cathodes so it must not have been that bad.

though this is something i had not taken into consideration when i was going to make copper nitrate. i think ill convert it into an oxide first and ill be more careful when adding acid to the solution to get a slower reaction.

Posted
From the papers I've seen on the matter, copper is plated in a 1:1 molar ratio with lead dioxide. We've been over this before, you wont be able to harvest a drop of nitric acid from the plating liquor, so I don't know why you're concerned with "losing" it.
Posted
darn, i was hoping to run the cell many times, to make many anodes with the same nitric acid used over and over again, so i would just need to dissolve more lead and copper for each batch.
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