Perchlorate production via electrolysis, with PbO2 anode
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- Опубліковано 17 кві 2021
- Process to produce NaClO4 and KClO4 via electrolysis by using lead dioxide anode.
You can buy the electrodes :
Just electrodes : www.ebay.com/itm/174220460094
Complete kit : www.ebay.com/itm/174663328746
Or just the lid : www.ebay.com/itm/174251053308
Or on my website : www.feanor-lab.com
To calculate the electrolysys runtime on my website : www.feanor-lab.com/calculator... - Наука та технологія
Awesome job here. You cover practically everything that causes trouble with perchlorate electrolysis. Chlorates are the easiest thing in the world. Getting rid of them is not; nice job on covering the required qualitative analysis. I use platinum anode myself but had a similar blocking issue.
Interesting thing is Sodiumperchlorate does desolve in Aceton, Sodiumchlorat doesnt, an way to seperate this two salts.
@@Preyhawk81 Well, it's sparingly soluble, not insoluble. I was taught that perchlorates with any chlorate contamination at all can cause problems, so I always use chemical methods myself to destroy residuals. Acetone might be a useful workup if you're starting with a really impure dried product. Even if your acetone is anhydrous it would still dissolve a non-trivial amount of chlorate, IMO.
can i use 10cm 0.3mm platinium wire?
Shoot I used too much persulfate and now the chlorate/perchlorate brine is very low ph. Is it buggered or can we increase the ph with something else? Sodium hydroxide perhaps?
Hi Feanor, thanks for the video.
i saw another video of kclo4 synthesis by thermal decomposition of kclo3. Is this good option to make kclo4 if have already have kclo3?
I never tried, but it is very hard, very high temperature, low yield, and need recristalisation from acetone. So if you need 10grams, it is probably good, if you need 1Kg, good luck 😋😉
Hello , Nice tutorial, is With this potassium perchlorate, do you can make whistle fuel, if you recristallise ? Maybe no? Thanks
Thank you !
Yes, of course you can use the potassium perchlorate for whistle fuel. If your first sodium perchlorate is quite pure, no need to recristallise KClO4 (who is almost impossible in water).
The pressing of whistle fuel in rocket is quite hard, (and dangerous) but the result is so impressive !
Love the video. Will these PbO2 anodes work for Kolbe electrolysis of sodium acetate to form CO2 + C2H6 or is platinum required?
Thank you !
For most of the applications, the PbO2 anode can suit to replace platinum, due to his high level of electrical potential.
The main constraint is the slow degradation of PbO2 xhich contaminate the solution.
I don't have knowledge for Kolbe electrolysis but if the contamination is not critical, I and your pH not above 10 or 11, I "think" it should work !
Feel free to share your own experience with us 😉
@@feanorforges I'm not too concerned about electrode degradation since I only need to do the reaction a few times. Main main concern is whether or not the catalytic effect of PbO2 is sufficient to release CO2 + C2H6 instead of just O2
@@HyperspacePirate In companies/universities labs, they almost always use Platinum anode for anything just because they have it and they have a lot of budget (platinum anode are very expensive), but most of the time, many other technologies are suitable like MMO (if you are a chemist, you probably know that IrO2 in my MMO has a highter electopotential than Pt) or sometime just nickel metal.
I really think your organic chemistry reaction just need a medium electrical potential suitable for MMO.
You can check on Ebay or on my website if you want where I have Platinum anode coated on Titanium (0.5grams/face).
Edition : I just checked on the internet, and yes, I can comfirm you that you don't obviously need PbO2 coating but it is more suitable if you have a very acidic solution, for medium pH, MMO anode is suitable forexample.
@@feanorforges Ok, thanks for letting me know
Chalk is the best way to neutralize sulfuric acid. Thanks. Nice tutorial.
Hey,there is one question.When you try to use indicator to test the chlorate ions in the solution, have you considered that sulfur dioxide in the solution may bleach the indicator. Maybe it could interfere with the concequence?
If indigo carmine reacted with sulfur oxides, then the result would be systematically bleached. By the way, it is not SO2 but SO3 which is produced firsly : Na2S2O5 + H2O 2Na+ + 2H+ + 2SO3 2 -
The confirmation of non-bleaching reaction of indigo Carmine can be found in US patent 2,392,769
When is the complete set going to be back in stock? I can’t seem to find some indigo carmine.
Hello, After a few days of getting perchlorate in my cell, instead of stopping, I continue to running it for another week or even more . Do you think it is a good way to get rid of residual chlorate in the cell? or does continuing electrolysis have no effect or benefit when perchlorate obtained? Soon I will making ammonium P.C with this method to see if its works or not but Again after using SMBS , the Ammonium Perchlorate what I got sharply smelling chlorine, than a few days later I seen the bottle get full of green Chlorine Gas.. I really don’t know how to can get rid of chlorate in perchlorate.. of course there is no single problem when I making potassium perchlorate but with ammonium chlorate existing its different, now I keep the bottle Inside a bucket full of water to avoid any possibility accident..
yes, your method is good it is my only one no, because destroying chemicals is not very conveniant as you seen, and not always perfect.
Run until 99.9% is not complicated BUT you need to control it to be sure, I put the other answer I let you on the video ot ammonium perchlorate :
"Don't worry, many of us, including me had a lot of trouble with removing chlorate and get pure ammonium perchlorate which don't smell chlorine gas.
Haha, no, you need to produce your perchlroate the same way than your usual method (MMO then PbO2), with 0.4% of persulfate if your cathode is in titanium (or chromate if in stainless-steel) and some times, you take a bit of brine, like 2 or 3mL and mix it with equimolar potassium chloride to produce KClO4. You make it dry and let drop a 30 to 36% HCl acid (commercial) and watch the color. If your perchlorate is slightly yellow : your perchlorate contains a bit of chlorate, but if your perchlorate remains white, you reached 99.9% perchlorate (congratulations), and thus, you could produce your ammonium perchlorate without danger, I do that, like Richard Nakka.
I can send you the colour reference for each purity with the HCl drop if you contact me on my website email.
(because the video won't be ready before 1 or 2 months at least, but it will include the total explications with this informations)"
Hi Feanor, is it better (efficiency or time wise) to go from nacl to perchlorate in one step using pbo2 electrode from the start or two steps nacl>cholrate>perchlorate ?
Always 2 steps, always, for tons of reasons ;-)
And what kind of power supply do you have for electrolysis? Where can one buy this?
fed
the salt creep losses are annoying and hence I usually run with a demister and completely sealed cell.
You would be surprised how much losses are owed due to the salt creep and mist because I legit have to put back 40ml of liquid a day which collects at the demister.
Yes, there are natural creep losses, but not so much. For each 600g of NaCl, I loose less than 20g/run and recycling it again. (you can put a dish under the cell...)
Sealed cell are really really complicated to build, the only way is glass + ptfe seal + pressure against + pipe for evacuation, in PTFE... (For long time I mean. For short ones, resin can be use for some weeks.)
Almost impossible for amateur, so the better way is to accept creep losses and put in the cell again, (or not ;-) )
@@feanorforges I just use rubber bands and some coat hanger wrapped around bottle and lid with wire and I use RTV silicone gasket by the recipe mixing with gypsum to make a putty.
This pressure mounted lid works well.
@@CatboyChemicalSociety I used silicone gasket too... but after 2 months it was dead !
@@feanorforges yea it does die but easily replaceable and cheap and overall 2 months is like nothing tbh thats just casual maintenance.
the blocking problem is something that really hits overall CE hard!! and idk what causes it but I heard its the additives in the feed salt and some say it is excess chloride in the left over feed.
I solve it by adding MgSO4 or magnesium persulfate and I did do a run without magnesium sulfate/persulfate and yea the yield was BAD and had to run for 2x as long without additives.
That's why perchlorates are not so much produced !
I think it is a series of chemical reactions at the cathode (and probably at the anode too).
Yes, the persulfate realy realy help the reaction process, many more than in chlorates.
And probably, the cathode coating of dirt can prevent the perchlorate formation, in my experience, I did restart a "blocking run" by polishing it...
@@feanorforges I never had problems with the dirt it doesnt seem to cause me any blocking since most of the reactions occur in the anode anyway. the cathode usually has things like reduction which counteracts the formation but any deposit would infact inhibit reduction.
@@CatboyChemicalSociety But you had blocking problems too...
And by the way, if the reduction doesn't work properly, the repercussion on the anodic process will be real ;-)
@@feanorforges I did yea but the blocking was fixed by forward feeding some NaClO4 if it does occur.
@@feanorforges Perchlorates are formed at the anode by oxidation of chlorate. My guess is if there is blocking at the cathode, if you are pushing the same current through the cell, cathode active areas have higher current densities. I think higher current density would correlate to more reduction of perchlorate back to chlorate or even chloride, thus reducing efficiency. I don't know about the persulfate. Do you know its method of action as to how it increases efficiency?
Is it possible to use Na2CO3 to remove acidity traces?
In my country, it's difficult to buy NaOH.
Yes it is almost the same, it is just softer and better for your security !!
But you should run until 99.9% perchlorate, you won't need to destroy chlorate, I'll send a video soon about this
Thank you so much!
I'm looking forward to your new video!
Hi Feanor, I'm busy making NaClO4 for other use and I'm wondering if additional NaCl could be added during the production proces given the very high solubility of NaClO3, and that the end concentration of NaClO4 could be made very high - if not precipitated out? You mention issues with recrystalization though, would this stop the process? Could more NaCl be added just to the NaClO3 production phase?
As far it is the chlorate run, yes, you can add NaCl it is what I'm doig myself, until 450g per initial liter of water.
But if you add too much, it crystallize at the bottom.
(one time you are in perchlorate run, you shouldn't, from my experience, but feel free to test, it is no dangerous)
@@feanorforges if solution Is costantly saturated with NaCl added using a basket for slow dissolution, you can precipitate directly the NaClO3
@@kingkama no, you will precipitate the NaCl only, I've tried many time, and always at the bottom, I harvested a crust of NaCl salt
@@feanorforges for me works, but you have to reach the saturation point and use a basket for the cloride so the solution Is ever full saturated. NaClO3 Is clear like ice and cristallize in big squared cristals
@@kingkama ok, it is another technics, I only use a saturated water to add, never tried a basket of chloride...
NaCl or NaLcO3 cristals are square too, but if you are sure, it is cool
hello .., i have a technichal question: should the cathode have less surface area than anode?? also why the need of pbo2 coathed anode for xclo4? any particular reason? also in the video of kclo3 systesis you choose double cathode surface respect anode counterpart...Others chemist suggest a lesser area for the cathode...so I am courious to understand better..THanks in advance :)
Hi, in industry, indeed, they often use smaller surface of cathode, so it should be a bit more effective or for some another practice reason (costs ?)
About the distance, it is for the electric yield (you can rise the voltage of 0.3V in some mm, so 0.3x30A = near 10W lost in heat for nothing) but about the chemical yield, it don't seems to change anything for me (yes, 7mm is better than 15mm for sure) but until 5mm it seems to be ok (I've no data below).
You should look in swiming pool electrolyser, some MMO electrodes are near 2 to 3mm spaced...
@@Baitrix1 In water but not in chlorate brine ;)
Is it possible to make kclo4 from potassium chloride with a pb02 anode and what material should the cathode be? thanks
No, it is not possible in practice because the KClO3 is almost impossible.
Some people succeed to melt KClO3 at high temperature like 400°C to get KClO4 but it is dangerous, complicated I never done it.
Electrolysis is more reliable and safe !
(the cathode can be in titanium, stainless steel, nickel, and other low corrosive metals)
Just a quick question the chlorate brine you used in the Perchlorate cell was it from a NaClO3 cell or KClO3? I watched your chlorate video and you used KCl. I already have a chlorate cell running and have everything ready I bought from you to start a Perchlorate cell just wonder about the brine.
My video could lead to confusion, I show at the same time the KClO3 and NaClO3 production but if you watch this video you could understand that only NaClO3 can be use to produce NaClO4 (the KClO3 is almost insoluble so...)
And overall, the sodium ions are better for the anode than potassium : the MMO anode will get a longer life.
@@feanorforges Excellent Sodium it is then. Thanks for this and for the quick reply. This is the most helpful and detailed video I've seen great work and thank you
@@webwarlock72 thanks, you are welcome !
What model of psu did u use?
After removing the chlorates with sodium metabisulfite and barium chloride, NaCl is left over. Does anyone know whether it is necessary to remove it from the sodium perchlorate solution? If it isn't removed, will it affect the use of the sodium perchlorate? Thx.
Oui, il faut le retirer le plus possible car il affecte l'efficacité du perchlo, ce qui se comprend aisément. Faire cristalliser l'ensemble, le NaCl cristallisera en premier au dessus du perchlo. Le retirer avec une feuille en papier en forme de tuile au fur et à mesure qu'il se forme. Refaire l'opération autant de fois qu'il le faut pour obtenir la pureté voulue.
so how do you get NaClO4 powder like you have at the start of the ammonium perchlorate video? do you even need metathesis ? keep doing electrolysis but use different anode after 1100 A/H/L ?
it is a bad example about the powder at beginning (I'll put another perchlorate video, more simple, and no need of metabisulfite and carmine).
The powder is just the ended brine, heated at 140°C to pass monohydrate to anhydrous NaClO4.
No metathesis for AP, just use NaClO4 from run.
And yes, the first run is done by MMO to chlorate, and then, to perchlorates with PbO2.
@@feanorforges I see the term some people use is crystallisation. An Aussie guy has a video with this. Yes no worries, sometimes difficulty is a good thing, given the sensitive nature ;)
@@VanKrumm You can only have NaClO4 monohydrate by cristalisation...
Yes, difficulties makes things valuable ;-)
@@feanorforges When can we expect this video? I'm very excited to see a method for obtaining pure perchlorate without metabisulfite. Greetings
@@Leo-mv7vh I'm ashamed because I'm very slow on this project...
but the process is simple, you continue the perchlorate run of electrolysis until a drop of concentrate HCl (33~37%) on a gram of KClO4 powder produced from the brine remain white. (near 99.8% and less 0.2~0.1% of chlorate).
The elecrical yield correspond at 21% more or less 2% but no need of chemicals to destroy the chlorate.
R.Nakka use this way too
Why not heat the solution up before starting the electrolysis?
Salut Feanor ! Pour l’étape de destruction des chlorates restant, comment faire si je n’ai pas de Indigo Carmine ? J’utilise quand même le Métabisulfate de Sodium « à l’œil » ?
On est obligé de détruire le chlorate de toutes façon (sauf à atteindre 99.8 ou 99.9% par électrolyse) , sinon le produit reste dangereux, et carrément obligatoire pour le passer en perchlorate d'ammonium qui dégagera naturellement un gaz chloré corrosif et asphyxiant, s'il y en reste !
Pour le métabisulfite, de toutes façons, il faut en mettre à l’excès, et plus simple que l'indigo carmin, c'est la goutte de HCl à 28~36% qui reste blanche sur une poudre que ne contient plus de chlorate mais devient jaune clair s'il en reste, c'est facile à voir, our de l'acide sulfurique 98% mais qui soit déjà transparente ce qui n'est plus facile à trouver de nos jours en dehors des labos.
@@feanorforges Merci pour ces précisions !
We need another video with more placement and subtitles
A new video is in production to reach 99.9% of perchlorate in one step without chemical destruction.
About subtitle, I'll add it when I'll have time
Now tell how do you make powdered aluminum with such small particle size, did you atomize it tho?
Under 8µm the "only way" is ball milling during many days, but the process is not so easy and quite dangerous.
Better to buy it directly.
how did you make the indigo carmine solution?
with water and hydrosoluble indigo carmine
Hello ! Tu as dis dans ton pdf que à la fin de la synthèse du perchlorate, il faut ajouter un peu de bicarbonate de sodium. Que arrive t-il si je n’en met pas ? Et est-ce vraiment nécessaire (ou puis-je m’en dispenser) ?
Merci
hello ! normalement, j'explique chaque étape.
Je parle de 3 perchlorates différents dans ce PDF, (que j'ai d'ailleurs mis à jour et que je suis en train de traduire, je vais mettre le brouillon sur le site en attendant, ça restera utile)
Je ne met jamais de bicarbonate à la fin de la fabrication d'un perchlorate, sauf éventuellement après la destruction du chlorate à l'acide, ce qui évite que la poudre reste acide et n'explose spontanément dans un feu d'artifice par exemple, en réagissant avec le soufre au autre composé sensible.
@@feanorforges Merci de m’avoir éclairé !
Just a thought but your reaction to destroy clo3 makes h2so4 as it seems from your formula so could you make 30-40% h2so4 from your metabisulfite method and high conc. clo3 solution in situ?
Some peoples use hydrochloric acid (HCl) to destroy the ClO3 but it is not very conveniant. Probably H2SO4 should works but always difficult to totaly remove at the end.
The question was If it´s a fast method to make strong h2so4 because it´s not easy to buy now. ClO3 + metabisulfite yields h2so4 from your formula. If you have saturated ClO3 solution you should get strong concentrated h2so4 right ? If you know better way please tell. It should be fast and easy. 30-40% h2so4 would be enough doesn´t need to be 98%.
@@Telectronics The answer is : I don't have feedback on H2SO4, just HCl so I can't be a good advice about it.
"Saturated solution of CLO3" ? no, if you want to clean you perchlorate you just have some percents.
In any cases, 98% is probably too strong for this aplication or useless.
40% is probably far enough.
@@feanorforges But it´s not my intention to clean perchlorate. Your formula says If you react clo3 + metabisulfite you get salt a sulfate and h2so4 right ? What have you to do to get maximum h2so4 right use full ammount clo3 + metabisulfite to get maximum h2so4 + sulfate + salt. Or am I wrong ? That is why I said saturated solution to use up a lot metabisulfite to get a lot h2so4. Sorry If I could not bring up that point. I hope it´s not dangerous to do that in small steps. I also need the h2so4 for anodizing aluminium and not to destroy the clo3.
@@Baitrix1 Sure If you can buy it...
wow!! very useful
Does only chlorate reacts with dyes and if so can we uses any type of dyes or just specific type?.
Actually iv been try to make colored smoke and for that i watched a lot of fake videos which use potassium nitrate as oxidizer but all my attempts failed then i read more about colored smoke i reach to potassium chlorate as an oxidizer for colored bomb but i cant make it but maybe i cane make sodium chlorate by electrolysis and finaly my last question.
Does sodium chlorate is good alternative of potassium chlorate for colored smoke or not? because i know that naclo3 stronger than kclo3
Nope, there is only few dyes which react with chlorate.
Nitrate are the best option for smoke production, most of the time, and you should watch at KNO3, sugar, paraffin which is well known and efficient. Chlorate are easiest to set off.
NaClO3 is very hygroscopic, so even if it is a bit better about oxygen giver, when your mixture is wet, it is a serious problem.
"Better" don't really mean anything, there are some mixture more efficient with KClO3, depend of reaction and purpose
@@feanorforges Thanks for fast response yes nitrate it gives huge thick mount of smoke but no color so if you know dyes or stuff for colored smoke mixture that will be very helpful 🙏.
@@user-mx6hd3vy5e You have lot of ressource all over internet !
For example, with chlorates :
ua-cam.com/video/EWaEhLhgeso/v-deo.html&
(36% Smoke Dye, 27% Potassium Chlorate KClO3, 18% Lactose, 19% Magnesium Carbonate)
with nitrate (KNO3) : ua-cam.com/video/_9Tkq3K1q_c/v-deo.html
(50% KNO3 + 40% Sugar + 10% Na-Bicarbonate. + Dye from Oil pastels + 20/25% )
NH4ClO4 is normally used to produce "colored" smoke.
@@user-mx6hd3vy5e The biggest issue I have found is that to get color (and actually a lot of smoke in general) the burn rate has to be suppressed by the retention of smoke within the device. The easiest way to do this is with a container that won't burn away and a small hole. Also keeping it cool seems to prevent the chlorate from detonating.
très bonne chaine jsp si c tout à fait correct en france mais très intéressant les kits que vous proposez on l'air assez complet mais je souhaite faire mes trucs moi même (c'est plus plaisant :) si vous voulez m'aidez de quelque manière que ce soit je suis preneur je suis amateur pour l'instant, en tout cas merci très complet et pas trop de blabla.
so what do you think of starting from KCl to make KClO4? the arguments i see with NaCl is that the solution has greater density of perchlorate and the run doesnt get clogged up with chlorate / perchlorate ppt.ing out
could current efficiency be lower too?
In fact, it is not really possible because one time your KCl is passed to chlorate, who is already crystalizing, you just have water and chlorate crystals... You can't continue the process... Maybe + some percent of perchlorate of course, but that is all.
If you feel that you can overpass chemicals properties, feel free to make a video ;-)
@@feanorforges oh yeah but chlorate is somewhat soluble with high temperature, i noticed with NaCl run, i would dump in excess NaCl and it would precipitate out NaClO3, and suck in more NaCl continously producing NaClO3
but i guess the KClO3 ppt'd out at the bottom is not gonna do much, as the perchlorate will ppt out ontop of that sealing it in
for perchlorate better is 10cm 0.3mm platinium wire or this pbo2 anode?
The platinium current density is near 0.4A/Cm² so your 10x0.03pi = 0.94Cm² = 0.376Amps against the 25/30Amps that could take this anode, the ratio is 80 times more productive ;-)
@@feanorforges please can give me your power supply name or link to buy?
Can i use sodium persulfate instead of pottasium persulfate?
Yes you can, same as ammonium persulfate, depends what is easiest to find
Can an MMO / Ruthinium / platinum combination be used for NH₄ClO₄ synthesis?
You're that guy who tries to electrolyze NH₄Cl in his bedroom aren't you? Go for it, what could possibly go wrong?
@@amarissimus29 Why, whats ammonium chloride got to do with the price of eggs?
@@Cornz38 Your question implies that you are asking if you can electrolyze an ammonium salt. I was being facetious because, assuming that is the case, you haven't read much about chlorates. If you are genuinely interested in the process, this is the last thing you want to learn, not the first.
You don't want to make ammonium perchlorate via electrolysis. Ammonium chlorate is very unstable and it would be even worse starting from ammonium chloride because you could get chloramines (that might actually be a danger going an electrolysis route no matter what actually). Ammonium perchlorate would be made by precipitating it from a more soluble perchlorate salt or via acid base reaction (which also has its own dangers).
@@kastonmurrell6649 Which is EXACTLY what i'm doing from sodium chloride then using a displacement with ammonium chloride.
Can you add persulfate from the very beginning (when electrolysing NaCl) and then run cell till the completion?
yes, but the anode lifetime is something like 3 times shorter in my experience, so I don't advise it !
@@feanorforges ok, thanks for advice
@@feanorforges isn't it what you've done here ? Doing the perchlorates following the chlorates ?
How much mmo i anod and how much pbo2 anod tell it reach to me in egypt I don't know how can be delivered to me
GO TO A POOL SHOP AND BUY MMO ANODES for chlorine generaters
This is great stuff. Where do you purchase PbO2 anodes? I've only ever saw them from China direct. No EU vendors. Still looking!
One day I will made a tutorial to show the anode coating process with lead nitrate... But as far the EU forbid nitric acid for private customers, they can't reproduce it 😕
@@feanorforges I am not a chemist but HNO³ is still realtively easy to aquire since nitrate salts are readily available. I've been reading a lot about depositing PbO² on Titanium substrates there on SM forum, but these most often explain it is a challenge to make the oxide layer adhere properly. You seem to have done the trick very well. The theory is there but in all the years I've been doing pyro, I've never attempted to build a perch generator. I envy those who succeed. Thanks for the vids.
@@JeffreyCC Esay ? Mmm, how do you get HNO3 from nitrate without sulfuric acid (banned last year) ?
Yes, you need some special MMO coating on the Titanium substrate before PbO2 coating, and it is the most difficult part.
@@feanorforges ua-cam.com/video/VLOY-Jp2w1I/v-deo.html
There is some usefull info in the comments. Using a mix of NaNO³ and KNO³ will lower the meltingpoint for instance.
@@feanorforges
You also might be able to obtain H²SO⁴ with the same equipment you are using to get your perchlorates by electrolysing a solution of CuSO⁴ in water. You will end up with pure copper and H²SO⁴
ua-cam.com/video/5dUSF9Gl0xE/v-deo.html
Can i use Road salt it is 98%> pure NaCl? The aditives are sodiumferrocyanide and potassiumferrocyanide. It is a anticaking agent
I strongly discourage you to use that, because many user sent me message to told me they get problems of pH and chlorine gas production.
Probably due to ferrocyanide but not confirmed.
The "pure" kitchen salt is near 0.25$/Kg and works very well 😉
@@feanorforges thanks for your quick anwser 🙏
@@feanorforgesWow thats some extremely cheap kitchen salt you got.
@@pika6238 haha ! Not you ?
@@feanorforges Cheapest NaCl here is .79 eur / kg :(
Hi, i've bought a few platinum anodes before and made NaClO4, but the part about the decomposition of Chlorate scares me the most..
Did that method of using Sodium Metabisulphite produce a lot of toxic ClO2 gas? Or has it ever done that in your experience?
Very informative video, thanks for sharing!
Hi ! Yes, it is possible : most of my customers who buy Pt anode coating are producing perchlorate !
The must is to study patents because they are using Pt anode in industry and cut the run at 50g/Liter of remain chlorate.
About chlorine gas, yes, all your chlorate will be destroyed, so all the chlorine will be release as toxic gas !
There are probably other methodes like solvents... I don't know.
(or you can heat the mixture over 300/350°C the chlorate will be destroyed and not the perchlorate who is 480°C)
Try to use that if you want : www.chlorates.exrockets.com/napermut.html
greetings
@@feanorforges Thanks for the soon response! I appreciate that..
I've tried decomposition of Chlorate with Hydrochloric Acid, but that's such a dangerous method as there's a very large amount of Chlorine Dioxide that can be released.. quite worse is that the mixture needs to be quite hot for the decomposition to progress..
Sodium Metabisulfite is one of the best methods, so I have read.. but I still want to avoid the use of Chlorine/Chlorine Dioxide gas... Do you heat your solution after your add the Sodium Metabisulfite??
Heating works, and as a matter of fact, just today I have tried thermal decomposition of crude NaClO4 (the NaClO4 cell liquor) to get rid of remaining chlorates and there has been so much chlorate it seemed, it took over 2 hours.. I've checked the temperature as well to make sure I'm not overheating it..
I haven't tried solvents, Laboratory of Liptakov has a video where he uses acetone to recrystallize..
Link: ua-cam.com/video/1Ylt2ZKJlME/v-deo.html
But working with acetone is difficult.
I'll try to use a lump-charcoal grill to heat my crude NaClO4 and maybe I'll do a video on it if it works because I'm sure there are folks out there who find it difficult with Perchlorate production and removing the remaining chlorates..
Again, wonderfully done video and presentation! Thank you and be safe!
@@reformlabs8742 Hi !
yes, I used hydrochloric acid, and yes, it is a cheap method but it works.
The "lot of chlorine dioxide gas" only happens if you have a lot of chlorate.
Good job for thermal decomposition.
I know the LL work : for 10grams it is ok, but not for 1Kg !!
You really should use PbO2 anode, to reach a pretty pure perchlorate liquor, like me, 99.5% and just destroy some grams of chlorate, it is really easier and quite safe.
Tell us if you try something interesting !!
@@feanorforges I'm quite impressed by the purity of your cell liquor! Very well done
I would purchase a PbO2 anode but my courier service mentioned to me that I cannot ship potentially toxic substances or flammable materials.
Unfortunately, I have to make my own PbO2 anode. Luckily my friend's dad had a 12V car-battery that's not working and he asked me if I've got any use for it (his dad knows me as the guy who has a use for almost anything) so they gave me the battery... I've picked it up today co-incidentally
I don't have much knowledge on PbO2 plating, I'll figure it out as I go along..
One guy used Lead Perchlorate, he left a comment below MysteriusBhoice but I still have to purchase a bit more apparatus as I don't feel very comfortable working with extremely soluble lead salts and since electrolysis tends to produce a sort of mist that gets everywhere, I would want to create a closed system to avoid the lead-electroplating solution from going everywhere..
I'm getting myself involved in electronics and programming so I could further build more advanced cells... and I'm hoping I can share it
I will however post a video up and be sure to send a link of a suitable thermal decomposition method (thermal decomposition also improves the yield) a mistake I made was that I did not use a catalyst like MnO2 so I'll try that when I have some more time to do so..
Anyways, I'm looking forward to posting something! Be safe and keep well
Warm Regards!
@@reformlabs8742 Thank you for your support !
I don't know where you are living but I have sent more than 200 anodes including many PbO2 coating who is legal for all countries that I know.
So far, it is OK for all European countries, USA, Canada, Latina america, Russia, Japan, Australia and NZ. Tell me is I can help you !
Yes, MysteriusBhoice try to produce Lead dioxide anode, and I'm waiting to see someone produce at least 1Kg with that.
Because it is quite easy to coating Titanium, but really more complicated to makes it durable in time.
You will probably do like me and 95% of amateurs: try, fail, and found other solution ! BTW, the easier way is to coat a graphite rod bar in rotation in lead nitrate bath, it is probably one of the accessible way for some amateurs, but most of the time it will work only for little batch.
If one day I have time, I'll probably do a tuto for producing this kind of anode, but it is just wandcraft, not really durable.
Tell me if I can help !
I created a cell of anode (positive) mmo, and cathode (negative) titanium, each of them are 5 cm * 15 cm, in a cell consisting of 2 liters of water added to them 200 grams of sodium chloride and I ran the cell on 5 volts and 20 amperes Within 24 hours, some rust appeared in the solution, and the titanium electrode turned black, taking into account that the temperature was maintained between 60 to 80 degrees. What went wrong?
please help me please
it seems normal. What it your MMO coating ? Ir-Ru ? And your cathode is just a little bit black ?
If your anode is in PbO2 coating, it is a normal thing.
@@Gabrielenegie Ir-Ru . Anode Coating
@@Gabrielenegie Does this mean that the anode is corroded?
@@AhmedSabry-cz4kf The Ir-Ru coating is black by nature, so you would mean the "Cathode" turned black ?
Did you put the + wire ont the Anode and the " -- " on the Cathode ?
@@Gabrielenegie yes + in anode and - in cathode
Can you use mmo electrodes instead of PbO2
It works a little bit but the life-span of your anode will be very short, and you can't reach 100% as PbO2 allow.
But I sometimes produced 20/25% of perchlorate and 75/80% chlorate... It is not very interesting appart to destroy visibly the coating.
is the chlorate brine you use in this video a freshly made one or is it the used one for the past video? can you start this electrolysis with a freshly made chlorate brine?
In this video, it was a old brine of chlorate finish some weeks ago.
But fresh don't change things, just the temperature help at the beginning to keep good pH and ions.
Probably fresh one, still hot is better to pass in perchlorate !
@@feanorforges so you just weigh a new mass of nacl in and use that as a starting point?
@@meesjanssen9206 No, I recommend to everyone by doing it in 2 steps, because 75% have trouble by trying passing from NaCl to NaClO4 in one step.
@@feanorforges thank you for you're help I really appreciate it!! Do you also have any recommendations in how you could clean the electrodes after the electrolysis?
@@meesjanssen9206 You are welcome !
For anode, I never clean them, for cathode, some use like isopropyl alcohol, but for me, I prefer sand it with sand paper, it seems to work well, but maybe it is not the better way...
Hello and congratulations.... I would like to ask your opinion: I have a cell with these electrodes powered at 5v and about 10 Amp of assortment after 4 days (at the beginning it absorbed about the later) I correct the PH daily with HCl to 6PH using a measuring instrument. How long approximately does it take for methylene blue to announce perchlorate? and approximately how long does it take to transform all NaCl into NaClO4? [I am not using any additives] thank you very much!!!.......and many more compliments

Thank you 😊
You have the calulator above, the last link in the description of this video, I let you play with the value, with the consideration of the yield that should be near 50% without additive. Ha, ok for transforming all NaCl to NaClO4 ? without additive ? near 15 billions years at least !😋🤭 haha no, sorry, you can't success for that !
But to pass all NaCl to chlorate, you can success but probably with 40% of electric yield in current.
Greetings
can i use sodium persulphate instead of potassium?
@@FCL-mp1zg yes, it is even better
@@feanorforges
do I throw the current brine? I corrected the PH always with HCL
@@FCL-mp1zg at which stage ?
Great video! Could you go more in deapth into the power supply. More than just linking a particular one: what characteristics should we be looking for
Thanks !
Depend of characteristics you are looking for. If you just send constant voltage, the currend will start from low, becam high and at the end will lower again. (if you don't want to invest and/or do it seriously, it is the better option)
If you send constant current, you will get high voltage at beginning and at the end, that will damage your anode.
Thus, it is important to have power supply with constant current AND limited voltage (example 5.5Volts).
@@feanorforges I have found one that looks exactly like yours and goes for quite cheap, it allows both current and voltage regulation. What wattage should I get? I see for your cell you are using a maximum of 6 volts and 90 amps
@@valfodr Your PSU wattage should be linked to your anode surface. (you understand that an anode of 100Cm square need other psu than 10Cm²)
You really should read my ebay's page and PDF about that, you'll have all informations.
And this PSU is 40Amps. The voltage is just a limitation, in good production conditions, for perchlorate, the voltage between electrodes would never rise above 4.0V but with a high current density, connection reistance and shape of anode, the voltage AT PSU could rise over, near 5.5/6VDC.
@@feanorforges Wow I had checked your eBay but totally missed the PDF. It's very exhaustive, thank you for the tips
@@valfodr I'm mounting my website which will be finish in some weeks, with more products than on ebay, and maybe PSU if people need, maybe some chemicals too :
www.feanor-lab.com
Can i use sodium persulfate instead of potassium persulfate?
Yes, totally ! It is probably a little bit better
@@feanorforges Ok, thanks
Молодец, где анод такой взял? Если сделал расскажи как или подскажи куда смотреть.
Спасибо !
Вы можете найти это в описании на Ebay или спросить меня напрямую.
Для изготовления он довольно длинный и деликатный, обычно из ванн с нитратом свинца или ацетатом свинца.
@@feanorforges хотелось бы видео увидеть как вы делали. Я делал на графите но результат так себе.
@@user-el8pl1pj3r У меня нет видео процесса, но я следовал этому руководству: www.chlorates.exrockets.com/leaddiox/leaddioxide.html
@@feanorforges спасибо, это уже что-то.
@@user-el8pl1pj3r Попробуй с диоксидом марганца. Говорят не хуже свинца и менее опасен для здоровья. Наносить проще. У Липтакова есть видео ua-cam.com/video/Xijper8WBPU/v-deo.html
0:43 What is A/H/L?
I imagine it stands for amp hours per liter
nice vid i love you ;)
Thank you Nich !
how did you get the chlorate brine?
By watching my video on chlorate production ;-)
@@feanorforges I did but is the solution you use in this video the solution you collected after the clorate reaction was finished?
@@meesjanssen9206 I took the time to explain all the stages in the videos, so if you can see the methylene drop becoming purple at the beginning of this video, it is to said that you have the answer (at 1:05) ;-)
Greetings
@@feanorforgesnow im understood why im always failed to make perchlorate, I always try to get it in one step from nacl.. so first need to make sodium chlorate than from chlorate to perchlorate:;;)
Hi guys 👋
My question is how i get potassium perchlorate crystals out of a potassium perchlorate solution? The Solution contains simply kclo4 and H2O. did i freez it boil it out? how exactly does it work and will it be pure kclo4 after getting rid of the water? Thank you very much.
As you can see, the KClO4 is barely insoluble and instantly form white crystals powder. You just need to filtrer with a simple filter, as a cloth.
But you should get rid of chlorate before cristallisation to avoid danger of uncontrollable reactions and self-ignition.
Im new in this field im just wondering, if per 100 ml at 0 degrees 0.76g / 100 ml is soluble in water if im dissolve 21.08g / 100ml at 100 degrees and it cools down to approximately 20 degrees room temperature, will there be 1-1.5 g per 100 ml in the solution and the rest sinks down as crystals?
Solubility of Kclo4:
0.76 g/100 mL (0 °C)
1.5 g/100 mL (25 °C)
4.76 g/100 mL (40 °C)
21.08 g/100 mL (100 °C)
@@highqualitypyro9075 Yes, more or less it is possible to do as you said, yes !
But this values are limits, in reality, we can't reach exactly this values in real !
@@feanorforgesthank you very much, I just find your documentary of electrolysis on your website :) this kind of detailed information is very rare to find 🙏🏻
Grettings from germany 👋🏻
@@highqualitypyro9075 I'm very glad that it could help you !
I'm on the preparation on another perchlorate video more simple without destruction of chlorate, just to run until 99.9%.
Greetings from France (and take care of you, pyro don't forgive 🙏)
interesting the persulfate additive, that is a good tip. Oxone is cheap freely available as well
Thanks, it is a good tip, the molecule is not too far from persulfate.
Right now, I'm leading some tests with Na-bisulfate it seems to works in addition with persulfate.
I have buy electrodes from him, and try anything for getting this product, but it not work at all.
Hello M.Bay, I'm sorry to hear that. Did you follow the video on chlorate first ? Tell me your parameters, I'll help you !
@@feanorforges yes many times i have see and read what you have sent to me. In you videos, you show kclo3 and kclo4 mixed, and its hard to find out what is going on there...
@@kennethbay2225 I'm sure you will succeed, for chlorates it is not very hard.
For KClO3 you just need to put a solution of potassium chloride, send 4.5Volts (for example) with your MMO anode and wait the apparition of KClO3.
For perchlorate, you do the same with table salt (NaCl), and stop the run when a drop of methylene blue become purple and then, pass it to perchlorate with your PbO2 anode.
Tell me at which stage you have problem
@@feanorforges It's the process that I can't get to work, no matter what I've tried, I can't get chlorate or perchlorate to form, even though I keep an eye on my Ph value. My desire is to form sodium perchlorate in one process, using double decomposition reaction. and I have bought both electrode sets from you, both for chlorates and perchlorates.
@@kennethbay2225 It is strange, because at least, chlorates are easy to produce.
One-step perchlorate is difficult, even me I don't do this anymore because it is easier and cheaper to pass by Na-chlorate first.
You really should to start with table salt, and wait the required time. With simple power supply, there are no many problems (even some guy succeed without persulfate, but pH is above 9, not good for electrodes an yield)
Hello, the pdf on your website that is for English has a page that is not translated to English, please check the file from page 19 to page 23 and a little in page 24. Other than that thanks for your hardwork!!❤
Thank you, yes, haha, you noticed !
I have to translate it and change it since September 2023 but I have 600 things to do, and I didn't took time, I'm too lazy, and can't stand myself hahaha !
I will try to update it in some days ;-)
thanks
Interesting process, but sadly not allowed in Germany.
allowed until 40%...
@@feanorforges okay, that's some dead weight, but maybe usable, thanks for the info!
calcium perchlorate is legal in germany like barium perchlorate from what I heard and that perchlorate can make everything including HClO4
赤熱したあと冷却された木炭を電極に使用する者がいないのはなぜ
Hello i need to your email