making potassium (per) chlorate

[WSM]

Quick question.

I ran a saturated solution of sodium chloride on 5volt and about 8A average for 6 full days, it was about 750ml and 1x4 inch platinized titanium anode and cathode, then i filtered it, boiled it to about 300ml (too much i think). I then added to it about 500ml of saturated potassium chloride solution, it started precipitating instantly, left it in the fridge for about 2 hours, filtered it off, re crystallized it and filtered at around 40c. I ended up with 220g of small white crystals.

What did i end up with? Lol

I got methylene blue coming in the mail i couldnt wait im doing things a55 backwards

 

Testing for chlorates is very useful, but it's trickier than testing for chlorides or perchlorates.

 

Chloride is determined by a silver nitrate solution, yielding a white precipitate.

 

Perchlorate is determined by methylene blue solution, yielding a reddish-purple color in the presence of perchlorates.

 

Both of the tests above use reagents that are reasonably stable in storage.

 

Chlorate determination is more challenging because of many things that can interfere.

 

I've used three different testing methods and none of the three use reagents that will last more than a few weeks without breaking down, so they don't store well at all, once they're made up.

 

The most reasonable method to use them is to store the reagents as dry materials and use miniscule amounts in a spot plate to test for chlorates. An exception to this is if you're doing lots of testing, making it more reasonable to make up a small batch of reagent and use it up before it goes bad.

 

WSM

Edited November 18, 2020 by WSM

[Arthur]

IIRC aquarium shops sell MB in solution here, please check in your state, regulations may vary.

[royster]

Yeah i dont know what it is it was a fun experiment tho, it seemed very potent when tested with fuels, my next move is trying to make some black copper oxide and making blue stars.

[Arthur]

Please check for chlorate content before being too experimental. Check out the incompatibilities of chlorates. Simply dont assume that your white powder is pure perc til you've tested it.

[royster]

Please check for chlorate content before being too experimental. Check out the incompatibilities of chlorates. Simply dont assume that your white powder is pure perc til you've tested it.

Thanks Arthur for reminding me to be safe.

 

I was going to try a chlorate and black copper oxide blue star composition that i found on this forum.

 

I did test it today, i dissolved a small amount in water and dropped 2 drops of methylene blue, it turned purple as it hit the water. With that im sure theres some chlorate and chloride in it so i am just going to treat it as chlorate.

 

I belive i read somewhere in this thread that theres a way to get rid of the chlorate, im going to get into that next time i run it.

[Arthur]

The important parts of the production process are (1)the separation of chloride from the chlorate at the end of the first electrolysis (because platinum electrodes can have a hard time with chlorides), and (2)precipitating only the perchlorate after the second electrolysis by adding KCl in calculated quantities.

 

Simply electrolysing the brine to perc will work BUT 1/ it stresses the platinum electrode (expensive!) 2/ there is no way to purify the perc so you end up with mixed perc with chlorate and hypochlorites which forms an unusable mix.

[xer]

In all posts that i have read there is a spectrum for current density on the anode(depending on material) like 80-300mA/cm^2 if you use lower current density i dont understand how you dont get any problems with overload on the powersupply ( im running into this problem) am i just overseeing something? any tips would be apreciated

[Arthur]

The current limit usually quoted is a safe running current above which the electrode surface will be damaged. Most of us want most product per electrode because electrodes are expensive to replace.

 

Once you have a cell and a electrode pair, you must work out the optimum current for best yield before electrode damage, then adjust the power for that current held steadily. For some people a cell may run for months, others only hours, so the cell must be stable enough for your intended use. If the available psu makes too much current then increase the length of the leads until the current is OK

 

The psu will benefit from being well away from the cell so that there is no corrosive mist spray ingested by the cooling fan

[xer]

Does a not submerged part of a Ti Cathode react with the gas mixture if so what does react there? i think TiO and TiCl need rly high temps i have seen formation of some brown rust like compounds in setups that allegedly use Ti as Cathode (maybe its just steel and they got ripped of)

[WSM]

Does a not submerged part of a Ti Cathode react with the gas mixture if so what does react there? i think TiO and TiCl need rly high temps i have seen formation of some brown rust like compounds in setups that allegedly use Ti as Cathode (maybe its just steel and they got ripped of)

 

 

If titanium cathodes or the leads appear to corrode,

 

1) be sure they're actually titanium

2) if they're titanium, be sure they're CP titanium and NOT an alloy.

 

CP titanium is "commercially pure" titanium with no or very little alloying metals in them (typically less than 0.5%), so we're looking at 99.5% or better titanium content. Many titanium alloys are available for strength, but we need the titanium as pure as possible for chemical resistance.

 

WSM

[Arthur]

Titanium has about as many alloys as steel! for heat for machining properties etc. The only metal we need is CP1 or CP2 titanium -both near enough pure for chemical resistance.

[WSM]

Titanium has about as many alloys as steel! for heat for machining properties etc. The only metal we need is CP1 or CP2 titanium -both near enough pure for chemical resistance.

 

 

Those two are good but I wouldn't rule out all the others listed as CP, if they're available to you. A simple Google search will likely result in a long list of titanium alloys available commercially.

 

I believe that CP1 is nearly pure titanium and easy to manipulate or machine, but it's not the only usable choice.

 

WSM

[WSM]

In all posts that i have read there is a spectrum for current density on the anode(depending on material) like 80-300mA/cm^2 if you use lower current density i dont understand how you dont get any problems with overload on the powersupply ( im running into this problem) am i just overseeing something? any tips would be apreciated

 

 

If we're talking about the process of making chlorates with MMO and titanium electrodes, they (high quality MMO) run well at 0.3Amps per square centimeter.

 

If the discussion is about converting sodium chlorate solution to sodium perchlorate, I had success using 0.1-0.2Amps per square centimeter on both platinum and lead dioxide anodes. I used a lab power supply capable of constant current (CC) operation and ran them on that mode for ease of end-of-run calculations. The same power supply for both tests ran flawlessly using an average of 4.0-4.5Vdc output. This was over four years ago (2016).

 

WSM

[xer]

 

 

If titanium cathodes or the leads appear to corrode,

 

1) be sure they're actually titanium

2) if they're titanium, be sure they're CP titanium and NOT an alloy.

 

CP titanium is "commercially pure" titanium with no or very little alloying metals in them (typically less than 0.5%), so we're looking at 99.5% or better titanium content. Many titanium alloys are available for strength, but we need the titanium as pure as possible for chemical resistance.

 

WSM

I know they got sold as material=Titanium no information on alloy or smth like that the submerged part doesnt corode but the cell isnt filled to the top because it would draw to much current and the psu would shut off only the not submerged part seems to corode(if i understand myself and you correct even the not submerged and not as cathode acting part of the titanium shouldnt corode right?(when its quite pure)) any way to check if its a titanium alloy else then the sellers description? thx for all the input

[WSM]

I know they got sold as material=Titanium no information on alloy or smth like that the submerged part doesnt corode but the cell isnt filled to the top because it would draw to much current and the psu would shut off only the not submerged part seems to corode(if i understand myself and you correct even the not submerged and not as cathode acting part of the titanium shouldnt corode right?(when its quite pure)) any way to check if its a titanium alloy else then the sellers description? thx for all the input

 

 

I fabricate my own electrodes (from bulk MMO mesh and titanium sheet metal) and I use CP titanium for my cathodes AND for the filled tubular leads attached to them in the cell. Even with all the salty vapor and splashing mists above the electrolyte causing salt crust on the titanium leads, I get no brown corrosion on them.

 

One remedy you might try is to clean and cover the leads with a compatible polymer material as a barrier to the salt spray inside the cell. If you don't have access to PVDF or PTFE shrink tube, you might experiment with wrapping plumber's Teflon tape as a proof-of-concept covering and see if it helps at all.

 

Let us know what you try and if it works.

 

WSM

 

Edit: If you try the plumber's tape experiment, use "half lap layers" meaning to carefully wrap a flat layer around the leads where the next layer covers the last layer by 50%. This effectively covers with two layers using one pass, and if carefully done will nearly seal the metal surfaces covered with a flat layer and not bunch up. Electricians use this method when applying vinyl electrical tape to wires or cables.

Edited December 6, 2020 by WSM

[PTFE]

hey all
Its a long time ago and many things where going on but finally i'Ve got something thrown together provisorily.

Its not the full 4Anodes+5Cathodes but 2 Anodes and 3 Cathodes in a 10l tank.

Planned is to run max. 200A but this time I did not implement active cooling as used in the small 125A version...We'll see if cold weather and a large tub of snow or water is enough to keep it below 95°C.

An dimroth willl be placed onto the vent to condensate the water. If needet, the cooling of the vapor could be turned of, to evapporate some of the electrolyte.






I hope you like it

 

Titanium has about as many alloys as steel! for heat for machining properties etc. The only metal we need is CP1 or CP2 titanium -both near enough pure for chemical resistance.

We also could use Grade7,7H,11,16,16H,17,26,26H,27 as they only contain palladium and ruthenium.

the grades 12,13,14,15 could also work but contain nickel and molybdenum

Edited December 28, 2020 by PTFE

[Arthur]

Oh yes I like it! You may like it for longer if you can protect the copper surfaces against corrosion.

[PTFE]

Oh yes I like it! You may like it for longer if you can protect the copper surfaces against corrosion.

thank you arthur

 

I had the same thoughts and will spray the whole top with clear coat, when fully assembled

[PTFE]

im really sorry for not participating for a long time. I will give you more informations and more pictures soon.
I also will read through the last pages when i'll find the time to do so.
Im quite buisy atm.

As i read on the last 2 pages, you discuss the corrosion of unsubmerged titanium parts.
I had run my 125A cell with the same 3 contact plates (- + -) for Years but i only had to replace the Cathode grids regulary as they corode due to heavy current loads. The contact plates though, which where the only parts not submerged for all runs, are fine as on the first day. Only the anode-plate got a nice golden color due to anodic passivation.

Im a but confused on how you get those corrosion issue.

Greetings,
PTFE

Edited December 30, 2020 by PTFE

[WSM]

thank you arthur

I had the same thoughts and will spray the whole top with clear coat, when fully assembled

 

A spray rubber coat may work well if it doesn't affect the copper.

 

WSM

[WSM]

hey all

Its a long time ago and many things where going on but finally i'Ve got something thrown together provisorily.

Its not the full 4Anodes+5Cathodes but 2 Anodes and 3 Cathodes in a 10l tank.

Planned is to run max. 200A but this time I did not implement active cooling as used in the small 125A version...We'll see if cold weather and a large tub of snow or water is enough to keep it below 95°C.

An dimroth willl be placed onto the vent to condensate the water. If needet, the cooling of the vapor could be turned of, to evapporate some of the electrolyte.

x (1).jpeg

x (2).jpeg

x (3).jpeg

x (4).jpeg

I hope you like it

We also could use Grade7,7H,11,16,16H,17,26,26H,27 as they only contain palladium and ruthenium.

the grades 12,13,14,15 could also work but contain nickel and molybdenum

 

 

CP Titanium with ruthenium (or an alloy of titanium with only ruthenium added) in it might make a great substrate for MMO anodes, or other electrodes.

 

WSM

Edited January 8, 2021 by WSM

[yardarmwheeze]

I think Nurdrage on YouTube had a good video on kclo3 not kclo4 though unfortunately. It involves electrolysis and the cathode and anode can be expensive the more quality you are trying to reach. (the process is super long as well)

https://www.youtube.com/watch?v=itAnVJ2vpHQ

 

You can also try to make kclo3 via boiling bleach but its really a waste of time with a crappy yield. If you are just doing it to mess around and you don't have the patience for electrolysis, then this might be for you.

 

Edit- Oops I had no idea how long this thread was...so I bet what I said was already mentioned..oh well lol

Edited February 26, 2021 by yardarmwheeze

[SharkWhisperer]

Like I said before--we're not trying to run you off--but we will not acknowledge or support stupidity and dangerous (and incompletely detailed) suggestions, That encourages taking shortcuts and guessing, which causes accidents.

 

Pyro/fireworking is inherently dangerous. There is no need to make it more dangerous. Boiling bleach? Smells great. And If you're too lazy to convert much more problematic chlorate into perchlorate then you're maybe too lazy to do safe fireworking.

Edited February 27, 2021 by SharkWhisperer

[yardarmwheeze]

Not "LOL".

 

You're wasting peoples time. People that you might learn a lot from but who don't want to deal with immature asses.

 

Segregate yourself from that group label with some smart, well-researched, considerate posts or queries.

 

Like I said before--we're not trying to run you off--but we will not acknowledge or support stupidity and dangerous suggestions,

 

Pyro/fireworking is inherently dangerous. There is no need to make it more dangerous.

Yeah I threw an edit in explaining how I didn't see how long the thread was. Obviously they already discussed what I mentioned, but electrolysis and boiling bleach are the two prime methods of synthesizing chlorate. Whether you like it or don't bleach with salt substitute is the most common quick and budget option of making chlorate. But your right I should've elaborated more on the second method. I thought that most people that read it would obviously have common sense not to do that in their house and do it outside or with a fume hood. But I will be more careful in the future, but what I said still stands. Those are two valid methods of obtaining chlorate

 

And please don't call me an ass or say that I would hurt animals. I respect your criticism but you always seem to lace your comments with a bit of malice or take it too far.

 

Also my book link was a book that I heard somebody mention, I never said it was any good or to read it. All I said was I caught wind of it from someone and I threw it out there as an option for someone to review. If you see my first topic I started, I mentioned how I knew a lot of things in chemistry and materials but I was new to actual fireworks and the art of pyrotechnics. I came to this forum to learn, but yes I should consult with a more experienced pyro on this forum before giving advice or info that I don't fully have experience with.

Edited February 27, 2021 by yardarmwheeze

[Arthur]

This is a monstrously long topic, it's been going for many years, every year some absolute gem is found among some absolute rubbish. It's hard but starting from the beginning is helpful to all who want to gain from the thread or contribute to it. However some of the original posters are no longer posting here and the wisdom researched and developed here may need regular refinement by new people with different sources and skills.