making potassium (per) chlorate

[WSM]

I'll do that then. I can't remember the voltage I was getting (chlorate cell),but IIRC correctly is was ~4.8-4.9V. I'm trying to find my notes...

 

A text book voltage for chlorate is 3.6Vdc and perchlorate is 4.0 - 7.8 Vdc depending on the set up and whose design you follow. Probably the electrode spacing has a lot to do with the workable voltage.

 

Give it a try and see what works for you.

 

WSM

Edited June 30, 2011 by WSM

[Bonny]

For this set up, I'm going to copy the electrode spacing I used making chlorate, about 1", as I intend to use the PC power unit. Making chlorate this gave me ~20A into the cell. I didn't get it set up yet, hopefully this week.

[lmodest]

you should really just buy it. its alot faster and more reliable

[oldmanbeefjerky]

alas, that is impossible, hydrogen peroxide will probably loose 90% of its oxygen before you reach 80 Celsius.

to purify hydrogen peroxide you must freeze it , which will cause the water (as ice) to precipitate out of solution, up to a certain point, i think that this can only be done up to 80% peroxide.

hydrogen peroxide has a freezing point of around -50 Celsius, so a standard freezer wont freeze it at all, also, sodium chloride will not mix into peroxide, if you allow a peroxide/sodium chloride solution to sit for a while, it will separate , like oil and water.

this is the basis of a simply peroxide purification instructable on instructables!

 

the acetates are about as ready as i can get them, and i will filter them off today (ive been busy due to cracker night and making fireworks to use on the day), i must though allow them to sundry outside, which wont be hard considering darwin at the moment is getting hot weather intense sun, and extremely low humidity!

 

in about 3-4 days ill post pictures of the powders, then the powders (once ive measured out enough copper acetate for all of the lead acetate i have), in solution being electrolyzed, and the electrodes stages of plating every 30 mins, though first i must get my hands on a suitable electrode to plate as i think i must use a large rectangular peice of metal for it to properly work, in which case ill buy some lead sheet from the local hardware store.

[WSM]

you should really just buy it. its alot faster and more reliable

 

Anybody can buy it (IF it's available to buy where you live, that is...), but where's the fun in that? If you can develop the skills and equipment to make it yourself from common materials, it leads to the satisfaction of self reliance and a much deeper understanding of the materials we work with to create our art. It's not the having of raw materials, but the search for knowledge and understanding which drives us.

 

I choose to expand my mind and skills...

 

WSM

[oldmanbeefjerky]

my view exactly!

i COULD go and pay $60 pper 250g of perchlorate, but i choose to do it for $1 instead

[50AE]

I'm tired of reading comment like "just buy it".

Some don't live in your contry, other neither in your continent!

[Arthur]

The whole point of the start of this thread, years ago was that perc, chlorates and nitrates are becoming harder to get retail in several places and in some places they never were retail. Swede put in a LOT of effort to find a way to produce perc if/when it becomes unavailable in the USA.

[Bonny]

you should really just buy it. its alot faster and more reliable

 

As Arthur noted, many people can't buy it. Plus if you do it right you can make your own as good or better than what you buy.

[oldmanbeefjerky]

i just came to realise i have only got 4-5 grams of copper acetate here, so ill have to do a bit more electrolysis with vinegar before i can start the electrolysis to make lead dioxide electrodes, also i gotta get a powersupply which can limit the amperage deliverd to the electrolysis cell because it apparently wont work otherwise. this may take some time. sorry guys, it is after all the first time ive done anything like this before, i wasnt prepared much.....

[Mumbles]

alas, that is impossible, hydrogen peroxide will probably loose 90% of its oxygen before you reach 80 Celsius.

to purify hydrogen peroxide you must freeze it , which will cause the water (as ice) to precipitate out of solution, up to a certain point, i think that this can only be done up to 80% peroxide.

hydrogen peroxide has a freezing point of around -50 Celsius, so a standard freezer wont freeze it at all, also, sodium chloride will not mix into peroxide, if you allow a peroxide/sodium chloride solution to sit for a while, it will separate , like oil and water.

this is the basis of a simply peroxide purification instructable on instructables!

 

the acetates are about as ready as i can get them, and i will filter them off today (ive been busy due to cracker night and making fireworks to use on the day), i must though allow them to sundry outside, which wont be hard considering darwin at the moment is getting hot weather intense sun, and extremely low humidity!

 

in about 3-4 days ill post pictures of the powders, then the powders (once ive measured out enough copper acetate for all of the lead acetate i have), in solution being electrolyzed, and the electrodes stages of plating every 30 mins, though first i must get my hands on a suitable electrode to plate as i think i must use a large rectangular peice of metal for it to properly work, in which case ill buy some lead sheet from the local hardware store.

 

You really need to even try to pretend like you've looked any of your information up.

 

You can only get to 62% by the freezing method. One inefficient, but somewhat functional, method of concentration is to heat it. Boiling it wont work, but you can kind of steam it off. 3% H2O2 boils at slightly over the boiling point of water, but at around 60C, the water will steam off more readily.. I've successfully concentrated 3% to around 22% (based on gas volume production via decomposition) via this method.

 

He was talking about chlorate + H2O2, not chloride. You also will want to start using real, credible resources if you want anyone to take you seriously. Indestructibles is laughable at best. Adding salt to a hydrogen peroxide/water solution will only give you salty hydrogen peroxide. NaCl solubility does lower with increasing H2O2 concentration though. You cannot salt out pure or more concentrated hydrogen peroxide.. Brine actually increases the solubility of H2O2 in water. The only way to really concentrate H2O2 is with vacuum distillation, and that is incredibly dangerous. (note the use of real references)

 

http://pubs.acs.org/...021/ja01313a064

http://pubs.acs.org/...021/ja01611a009

[oldmanbeefjerky]

hmm, well perhaps i misread, though i swear the pictures taken showed the peroxide seperating from the salty water. well, it seems i was wrong, so nobody listen to what i said before, it seems the instructable was faked!

 

also,

i just filtered the copper and lead acetate (removed the solid metal lumps), and now must allow them to naturally evapourate, its times like these when i consider building a vacume boiler / desicator !

and i have been meaning to build a pump too for my distil....... ive taken pictures though its not really much to look at, just a plastic cup with a tablespoons worth of lead acetate crusted on the rim, and a clear cup of blue water. though ill post it all on my slideshow, and will soon begin documenting it onto my website since it hasnt yet been documented elsewhere for the same outcome as i want , which is to create lead dioxide electrodes.

 

-edit-

 

word of warning (from personal experience) :

when making lead dioxide electrodes via electrolysis of sulfuric acid with lead electrodes, make sure than no copper (like say from the wires attached to the lead electrodes), does not contact the acid, or else it will form copper sulfate which will be plated on the catchode which is supposed to be plated by lead dioxide, but so long as there is copper sulfate, the cathode will be plated by copper. quite effectively too, i have a solid 0.5mm layer of copper now on my lead dioxide electrode, which looks rather nice, besides, the copper layer will come off soon enough on its own when i use it to electrolyse salt water in a hope to make sodium chlorate.

Edited July 6, 2011 by oldmanbeefjerky

[pdfbq]

you should really just buy it. its alot faster and more reliable

I am also getting tired of these comments. You also can buy firework, so what's the point making it? Edited July 6, 2011 by pdfbq

[oldmanbeefjerky]

exactly!

i myself dont like to go throwing money around on things i can easily make as it was put before, the same or better that retail, though i myself have never managed to make a batch of chlorate that ever worked, as i know very little of the science behind it

Edited July 6, 2011 by oldmanbeefjerky

[WSM]

... though i myself have never managed to make a batch of chlorate that ever worked, as i know very little of the science behind it...

 

OMBJ,

 

See if you can get one of lasered's eBay electrodes (MMO coated CP titanium mesh) and a nice piece or two of CP titanium sheet metal roughly the same size. Properly connected with a decent power supply, you can make all the chlorate you can handle (and then some...) ! There are none listed at the moment but they appear from time to time at decent prices (check out item number 330580676075 or better yet 260806797107 for instance).

 

If you need guidance utilizing any of these, several here have experience they're willing to share, if your goals are honorable (fireworks or rockets; not mischief ).

 

Beware of copper salts in a chlorate cell (likely creating copper chlorate which is something to avoid at all costs).

 

WSM

[oldmanbeefjerky]

"CP", what does that stand for anyway?

 

yes, my attempts are honorable, in a way, i need chlorate to make coloured smokebombs, which is impossible to achieve with potassium nitrate as it burns to hot and destroys the smoke mix

 

these electrodes though, what exactly is the MMO composition on them?

 

i soon plan on making titanium plated electrodes as a family member overseas's job is cutting massive ( 20M cubed more or less) pieces of titanium for companies to use (for what though i haven't a clue), and when i told him i was starting up an online store, he suggested i use some of the titanium shavings, which i later discovered were very large shavings, 3 x bigger than a standard ruler in all dimensions more or less, as people may be interested in buying them.

 

lastly, since i have looked over a hundred times for titanium electrodes and anything really which is useable, and came up with squat, what are these "decent prices"? as i have no idea what the standard eBay value for such electrodes are!

 

 

this also brings on another question, as i have come to realize, MMO can mean cobalt manganese oxide, made by decomposition of cobalt and manganese nitrate in an etched titanium plate, who here has ever used such electrodes, and how long to they last, because if they do last rather long, i might make an investment in buying some of those compositions to make my own, to also sell.

 

hopefully though LD electrodes work well enough for me to forget about any of these other ones!

and if the ones i have already built work, then it will be a simple matter of re-electrolyzing them in sulfuric acid every now and again when the lead dioxide coating wears off, as it only takes a few hours to grow back during sulfuric acid electrolysis.

Edited July 6, 2011 by oldmanbeefjerky

[Mumbles]

CP stands for chemically pure in most cases, sometimes commercially pure.

 

MMO literally means mixed metal oxide. Often times the composition is proprietary. I'll try to find the paper again for making them specifically for chlorate and/or perchlorate production. I believe it was about an even mix of Titanium oxide, ruthenium oxide, and sometimes one more (lead, tin, iridium, tantalum usually). The ruthenium chloride starting material runs about $9/gram depending on quantity and source. Ruthenium acetate isn't really what you would imagine, and is probably useless for this application. It should probably also be mentioned that MMO isn't electroplated, rather painted and then baked on repeatedly.

 

I hope you're doing your homework on making these properly and are intent on delivering a quality product, not just something that you think is good. Bad electrodes can put people off of the research.

[oldmanbeefjerky]

well, lead dioxide would make the most sense , or iridium, considering how close to platinum it is, also dont worry, im actually going to test out these electrodes and make sure they really work before i even consider selling them.

 

also i know how MMO electrodes are baked, i saw nurdrages video on making the manganese and cobalt oxide electrode. i hope i wont need to obtain any of the nitrates of those compounds (titanium, ruthenium , lead, tin ,iridium, tantalum), because i wont have access to nitric acid for another year or so, because no-one stocks nitric acid in the northern territory, which sells publicly like in Queensland, and i dont look forwards to making sulfuric acid from my copper sulfate just to make a small amount of nitric acid from my potassium nitrate! especially without proper electrodes to electrolyze the copper sulfate with!

Edited July 7, 2011 by oldmanbeefjerky

[WSM]

"CP", what does that stand for anyway?

...what exactly is the MMO composition on them?

 

Hi OMBJ,

 

CP titanium is "commercially pure", and basically un-alloyed titanium. The one description I recall of MMO used for chlorates (MMO doesn't work for perchlorate but can be a good substrate for LD which does work for perchlorate) is about 70% TiO₂ and 30% RuO₂ on CP titanium. An MMO anode with C.P. titanium cathodes works well for a long time making good, clean chlorate.

 

WSM

[oldmanbeefjerky]

ah excellent, and i presume that i will be getting the titanium and ruthenium painted and baked ( i wish i knew the process name) in the form of nitrate correct? ( as in paint with nitrate and bake it to decompose into oxide) or will some other form work also? e.g acetate ?

i really dont want to have to go and make nitric acid just to end up destroying it!

 

also, correct me if im wrong, but isnt titanium dioxide unconductive? or does it serve more as am inert bonding agent?

Edited July 7, 2011 by oldmanbeefjerky

[Mumbles]

Perhaps you should spend some time reading up on if all of those chemicals you're asking about exist (I of course mean real world, bulk quantity, exist), how to make them, if they're stable in water/air, and the process by which to make MMO electrodes.

 

Titanium dioxide, presumably dependent upon crystal structure, is a semiconductor.

[oldmanbeefjerky]

oh i already know where i can get all of those, i recently did a big search on chemical suppliers a while ago in my search for 5kg of copper sulfate which costed less than $30, and i found out that i have a local chemical supplier 20 minutes from my house, and they stock pretty much everything.

and also there are many pottery raw chemical suppliers in queensland which sell bulk amounts of many different oxides such as tin, titanium , cobalt, nickel and manganese all of which in very very large amounts, and i know that for the cobalt and manganese electrode which does work well for chlorate, it at most only needs a teaspoon of manganese and cobalt!

 

also, all of these have a nitrate form, and to make an MMO electrode, is simply a matter of decomposing the nitrate in layers, on the electrode, as nurdrage did in his MMO electrode video .

 

 

by the way, has anyone here every tried using a pool chlorinator anode and cathode pair for making chlorate?, i read up that its possible in small amounts (250 grams/L) at a time but will not make any perchlorate nor will it survive being run a bit over 1 amp! is this true?

i may consider salvaging these and plating them (they look just like the platinum titanium electrodes ) in lead dioxide or if possible or a layerd mix of lead dioxide and cobalt if it is at all possible using lead and cobalt nitrate to do so, rather than electroplating, as electrplating would most likely end up clogging up the mesh, resulting in many weakpoints for the electrode!

[Mumbles]

From what I've read cobalt doesn't stand up to perchlorate what-so-ever, and has a fairly limited life in chlorate. Perhaps mixes hold up better. Some of the others seem to be a bit better.

 

I feel that NurdRage's method is limited in several ways compared to the ways it's done commercially. The layers look to be extremely uneven, and probably not all that durable. Often times there are additives added to the solution to increase viscosity to allow better coating, and the temperatures/environment used is much more controlled and often significantly higher.

[oldmanbeefjerky]

i agree, but at the moment its all i can get my hands on without spending $300-500 on about 75g ruthenium.

 

after considering all the other possibilities, i think that i will be best off just using lead dioxide! i already have one electrode i have made, though it does have an extremely thin coating (just lead electrolysed in sulfuric acid), so ill have to see how long it will last before i go and get/make some lead sheet to get an electrode with a higher surface area to minimize corrosion, perhaps i will consider plating pool chlorinator anodes with lead!

Youve had experience with lead dioxide yes? on a rough estimate of pure lead dioxide electrodes, how fast do they corrode when making chlorate and perchlorate at the voltages and amp's at which you use them? im finding it very difficult to source information on this.

[WSM]

i agree, but at the moment its all i can get my hands on without spending $300-500 on about 75g ruthenium.

 

after considering all the other possibilities, i think that i will be best off just using lead dioxide! i already have one electrode i have made, though it does have an extremely thin coating (just lead electrolysed in sulfuric acid), so ill have to see how long it will last before i go and get/make some lead sheet to get an electrode with a higher surface area to minimize corrosion, perhaps i will consider plating pool chlorinator anodes with lead!

Youve had experience with lead dioxide yes? on a rough estimate of pure lead dioxide electrodes, how fast do they corrode when making chlorate and perchlorate at the voltages and amp's at which you use them? im finding it very difficult to source information on this.

 

Hi OMBJ,

 

I think the most efficient way to get MMO is to buy it unless it's totally unavailable or you need a custom shape. I think making MMO when you can buy or harvest it (as from pool chlorinators), is comparable to a whisky distiller looking for copper ore to make copper tubing for a still rather than focusing on making the product (whiskey). I looked up lasered's shipping rate to Oz and the 10" x 6.75" MMO mesh would cost you about $25US delivered. Even if you hacksaw the piece in two and bolt electrical leads to the MMO mesh, leaving a fair bit out of the solution; it would make a LOT of chlorate (tens of kilos, at least and probably more). I imagine you could use one of the halves to plate with LD and convert some of the surplus chlorate to perchlorate.

 

Unless you love the process of making electrodes (in which case I'll keep my peace and cheer you on) I'll keep offering suggestions on how to obtain them without the challenge of making them.

 

WSM