Sodium Perchlorate synthesis from NaCl to NaClO4 using lead dioxide electrodes. 

This is electrodeposited PbO2 on DTO coated titanium where DTO is baked doped tin oxide as you cannot plate it directly on titanium. The lead substrate PbO2 is limited in use case and corrodes more readily than the titanium subatrate version

@@CatboyChemicalSociety is it possible for the pb+pbo2 anode to survive in a perchlorate cell? im guessing not but ill ask just in case

@@ouepillthegoat no it will fail due to interface oxidation of Pb substrate by hydroxy radicals. The electrode used in the video is homemade using Ti substrate and DTO coating which ive shown previously then PbO2 deposition using alkaline medium.

Many huge mistakes here. Firstly you should have only used one anode and 2 cathodes because to run a perchlorate cell you need 150ma/cm² on the anode. Also 70C is too hot and you need water cooled glass cell. If I assume your anode is actually 130cm² accounting for both faces meaning the electrode is about 5x15cm which roughly gives 150cm² so its more like 5x13cm. Anyway 130x150 = 19,500 ma so each anode is rated at 20 amps with 2 cathodes for even CD loading. For 2 anodes you need 40 amps to run it with 3 cathodes and a fkton of water cooling or heat exchanger see my latest video. My suggestions to you is switch to glass.3 liter cell. Use 2 cathodes not titanium because its terrible without buffers and use graphite or stainless instead. Run at 20 to 25 amps and keep temperature below 55C. Also if you want to fix your anodes see part 2 or 3 of my PbO2 from DTO video.

@@CatboyChemicalSociety Thanks for the quick reply . The anodes is 15x10 . But it is a titanium mesh that's why I reduced 20 cm2 . But I think I only calculated the surface aria for one side.

@@kasrah.2087 15x10 then each anode needs 40 amps. Really go watch my video on water cooled perchlorate cells because otherwise your anode is too big. The minimum current density for PbO2 is rly 150ma/cm² and is also nice to run for the 55% efficiency with sharp drop off lower than it. A current density of 200ma/cm² gives an efficiency of 87% and is good if the anode is layered composite PbO2 which it isn't. The 2 most important equations is the surface area of a double open ended cylinder since coolant usually is annular and fourier's law of heat conduction is the second equation.

@@CatboyChemicalSociety Thx bro .I'll report my next atempt

@@kasrah.2087 if you ever damage those electrodes beyond repair then you can recoat them using my DTO substrate PbO2 videos

Your power probably 5 volt 2 a, 100 120 ml hot water probably enough for dissolving sodium chloride. For this volume of water and this gram salt. I can say after 24-48 hour enouhh

I think your solutions were too concentrated and for this synthesis you must ensure that its dilute otherwise barium sulfate wont go out that much. After preparing about 30% perchloric acid and filtering off the barium sulfate you can then boil off the water or distill it off whichever then this gives you 70% perchloric acid.

@@CatboyChemicalSociety thanks, I had added acid straight to solid, I'll try adding some water, heating and filtering it

@@SodiumInteresting adding sulfuric to straight solid is a good way to BLOW UP. anhydrous perchloric acid is FUCKED and really dangerous and can spontaneously detonate.

@@CatboyChemicalSocietyI kept quantities small. Probably good I didnt use oleum. I added small amount of water and it's gone cloudy with a clear bit on top, at the bottom is white solid which seems like different substance to the starting material.

@@CatboyChemicalSociety I appreciate the warning btw

Do not leave electrodes without current or it may but not always cause galvanic reduction of the anode. This will however happen if left unpowered for 6 hours or more.

PbO2 cannot be left unpowered even for 30 mins as it's very prone to galvanic effects.

45 euros for these 5x10 cm rated at 20 amps

its an alpha PbO2 coating process so nope. and if it was beta PbO2 the most they do is add layers of alpha PbO2 or have carefully controlled temperature curves to destress them with both these working. Alpha PbO2 is free from stress but overcurrent above 250ma/cm^2 is not good for it.

Can i use lead oxide instead of lead dioxide for perchlorate electrolysis thanks

homemade but making it is a pretty complex process.

@@CatboyChemicalSociety Meh... I've got plenty of large reaction vessels, a whole machine shop, and some pretty solid power supplies... I've been doing various random chemical reactions since early childhood, and now after years working in renewable energy research, I've pretty much developed a good enough sized laboratory that not much is out of my reach even without buying any new equipment. Complexity is not an issue for me. I just need to know I am doing it the best possible way I can and I'll be quite pleased.

@@hunnybunnysheavymetalmusic6542 basically you would need an DTO or MMO substrate which is a mix of tin tetrachloride and any dopant like ceric chloride 8:2 ratio and you can use the pentahydrate so it doesnt fume and is easier to synthesize with my latest video on it. Then you must plate PbO2 at 2.3ma/cm^2 with a saturated plumbate solution at 50C constantly with strong stirring for about a day or so.

@@CatboyChemicalSociety Cerium is a mineral found in this area where I am, so its possible I could manufacture my own ceric chloride in situ, and tin is super easy to get from recycled electronic scrap, so that's nothing but a little recycling... I'm really encouraged, because with all the insane restrictions these days on oxidizers, and my aims to get into full scale mining, its really a total game changer to be able to produce my own perchlorate on site, instead of going through all the garbage to get permits and buy it and all that garbage.

@@hunnybunnysheavymetalmusic6542 the cerium has to be pure enough

the surfactant is eventually destroyed though. so it needs to be dosed more after some time. I notice because even the bubbles dont overflow it eventually stops producing foam after some time. The scrubber liquid can be either MnO2 or urea or a mix for decomposition of ozone.

SnO2 coatings are better

​@@CatboyChemicalSocietyI need you to answer my question: How much time do I need to convert 100 grams of sodium chloride into perchlorate using graphite electrodes and mobile charger.

@@hzjddhjs9313 graphite will disintegrate and oxidize to CO2 before it makes any perchlorate go get a proper electrode and psu. It will take a month to get to chlorate full conversion.

this thing produces an ungodly amount of ozone which is why the scrubber was warranted and even with a scrubber the ozone smell persisted albeit in ok levels like an electronic shop and not sticking nose into high voltage source.

@@CatboyChemicalSociety I still really appreciate that taste of a lethal dose of radiation

@@CatboyChemicalSociety Platinum and lead dioxide electrodes are both used in the electrolytic production of ozone from dilute H2SO4 solutions, iirc they can produce up to 15% ozone in the oxygen released at the anode. Definitely wise to run it through a scrubber.