Jump to content


Photo
* * * * * 5 votes

making potassium (per) chlorate


  • Please log in to reply
5357 replies to this topic

#41 LGM

LGM

    Pyromaniac

  • Full Member
  • PipPipPip
  • 106 posts

Posted 15 August 2007 - 09:56 AM

Don't hold me to this but I think that the tungsten will corrode if used as an anode. If you already have some then go ahead and try it, but I have never heard of it as being used for this.

#42 Tweetybird88

Tweetybird88

    Pyromaniac

  • Full Member
  • PipPipPip
  • 151 posts
  • Location:USA
  • Interests:Fishing, hunting, pyrotechnics, chemistry

Posted 22 September 2007 - 05:04 PM

You are probably going to hate me for resurecting this thread but I think this would be a really fun project for me. My first questions are: how do you make the anode with platinum wire? and where do you get sodium chlorate? Is it still used as herbacide?
  • abbykarim and deepakpyro like this

#43 frogy

frogy

    Pyrotechnician

  • Full Member
  • PipPipPipPip
  • 360 posts
  • Location:Kent, Ohio
  • Interests:Pyro, gaming, computers in general, paintball, potato guns...

Posted 22 September 2007 - 05:46 PM

I think your a little confused... hehe
It's not Sodium Chlorate it's Sodium Chloride...

Potassium Perchlorate
----------------------
NaCl -> NaClO3
NaClO3 + KCl -> KClO4

Potassium Chlorate
----------------------
KCl -> KClO3


Sodium Chloride is common salt... I'm not sure if road salt is pure, but it's probably the cheapest source...

I believe Potassium Chloride is what is used as a water softener... Or it is known as "potash"... Not really sure

Sodium Chlorate is a decent oxidizer already... And your right, it is a herbicide

#44 Tweetybird88

Tweetybird88

    Pyromaniac

  • Full Member
  • PipPipPip
  • 151 posts
  • Location:USA
  • Interests:Fishing, hunting, pyrotechnics, chemistry

Posted 22 September 2007 - 06:00 PM

I think your a little confused... hehe
It's not Sodium Chlorate it's Sodium Chloride...

Potassium Perchlorate
----------------------
NaCl -> NaClO3
NaClO3 + KCl -> KClO4

Potassium Chlorate
----------------------
KCl -> KClO3


Sodium Chloride is common salt... I'm not sure if road salt is pure, but it's probably the cheapest source...

I believe Potassium Chloride is what is used as a water softener... Or it is known as "potash"... Not really sure

KCl is water softner and it is extremely cheap. I saw it at the supermarket for superlow prices. I didn't know that sodium chlorate waseasily produced from salt so I thought you had to get that first. I'm in my preliminary research for this chem expiriment and am very excited for it. But I still have my question from before. How do you make the anode from wire? Do you just coil it around a tube? I've seen pictures but am not really sure what they did.

#45 WarezWally

WarezWally

    Pyrotechnician

  • Donator
  • PipPipPipPip
  • 701 posts
  • Location:The land down under

Posted 22 September 2007 - 06:58 PM

Just coil the wire and place it in the solution.

#46 frogy

frogy

    Pyrotechnician

  • Full Member
  • PipPipPipPip
  • 360 posts
  • Location:Kent, Ohio
  • Interests:Pyro, gaming, computers in general, paintball, potato guns...

Posted 22 September 2007 - 07:22 PM

Alan Yates coiled it around a glass tube... I suppose you could just coil it and put it in the solution through the lid though... It would probably have more surface area...

Posted Image
  • abbykarim likes this

#47 hashashan

hashashan

    Pyromaniac

  • Full Member
  • PipPipPip
  • 164 posts

Posted 23 September 2007 - 02:08 AM

I think your a little confused... hehe
It's not Sodium Chlorate it's Sodium Chloride...

Potassium Perchlorate
----------------------
NaCl -> NaClO3
NaClO3 + KCl -> KClO4

Potassium Chlorate
----------------------
KCl -> KClO3


Sodium Chloride is common salt... I'm not sure if road salt is pure, but it's probably the cheapest source...

I believe Potassium Chloride is what is used as a water softener... Or it is known as "potash"... Not really sure

Sodium Chlorate is a decent oxidizer already... And your right, it is a herbicide

What drugs did you use today?
NaClO3+KCl = KClO4??????:? WTF??

NaClO3 ->electrolisys at certain conditions -> NaClO4

NaClO4 + KCl = KClO4 + NaCl

and potash is potassium carbonate not the chloride, the chloride is what is called low sodium salt.
  • SharkWhisperer and MikeL like this

#48 WarezWally

WarezWally

    Pyrotechnician

  • Donator
  • PipPipPipPip
  • 701 posts
  • Location:The land down under

Posted 23 September 2007 - 03:29 AM

I'm confident with the whole procedure (at least the chloride to chlorate side of things) but how do you remove or destroy sodium chloride? (assuming you use NaCl as the starting salt).

With my potassium chlorate i made i couldn't let the chloride level drop to low or the graphite anode would erode very quickly thus when i did the double decomposition with KCl the yielded KClO3 was heavily contaminated with NaCl pretty much making it useless. I havent seen anything about this (or i mentally skipped it), any ideas?

btw, has anyone had any luck getting a commercial TSLD or GSLD anode? I did send off a email to a place in the UK asking for prices for about 10 anodes but i never heard back.

Cheers

#49 hashashan

hashashan

    Pyromaniac

  • Full Member
  • PipPipPip
  • 164 posts

Posted 23 September 2007 - 03:55 AM

Many recrystalisations would make a pretyy clean K-Chlorate.
However if you are not after perchlorate then the best way is to make the Chlorate out of KCl.
If you want to make some perchlorate then you have two choises. Either make the direct perchlorate from chloride using PbO2 otr get pure chlorate(very very very low chloride) and then use platinum.
You can get pretty pure Na-Chlorate form K-Chlorate(using many crystalizations) by this way : 2KClO3 + Na2SO4 = K2SO4 + 2NaClO3 at hot temperatures and then add some EtOH to precipitate the K-sulfate, if anyone is interested i can put here the whole process.
  • tortoise likes this

#50 Tweetybird88

Tweetybird88

    Pyromaniac

  • Full Member
  • PipPipPip
  • 151 posts
  • Location:USA
  • Interests:Fishing, hunting, pyrotechnics, chemistry

Posted 23 September 2007 - 06:45 AM

So let me get this straight. To make potassium perchlorate I would start with sodium chloride change it to sodium chlorate and then the sodium perchlorate and then add potassium chloride and end up with potassium perchlorate.
  • Sulphurstan likes this

#51 '''

'''

    Playing with fire

  • Full Member
  • PipPip
  • 23 posts

Posted 23 September 2007 - 06:52 AM

Exactly :D .

#52 Tweetybird88

Tweetybird88

    Pyromaniac

  • Full Member
  • PipPipPip
  • 151 posts
  • Location:USA
  • Interests:Fishing, hunting, pyrotechnics, chemistry

Posted 23 September 2007 - 07:19 AM

OK in that case, I will start with just potassium chlorate. What is the best anode to use for making chlorates? I heard that titanium will corode pretty good when making chlorates and is not worth the expense. Should I use lead oxide? The cathode is best as titanium in both cases if I am not mistaken. And to make chlorate it is just potassium chloride---->pot. chlorate.

#53 WarezWally

WarezWally

    Pyrotechnician

  • Donator
  • PipPipPipPip
  • 701 posts
  • Location:The land down under

Posted 23 September 2007 - 09:25 AM

Yes. Titanium is cheap, I picked up a large sheet for $10. Lead dioxide will make the best anode.

#54 frogy

frogy

    Pyrotechnician

  • Full Member
  • PipPipPipPip
  • 360 posts
  • Location:Kent, Ohio
  • Interests:Pyro, gaming, computers in general, paintball, potato guns...

Posted 23 September 2007 - 09:34 AM

Potassium Chloride + Electrolysis -> Potassium Chlorate w\ Potassium Chloride

I believe you dry the KClO3\KCL crystals and then add that to water and boil off the KCL...

I've always wanted to make a cell for this (I have some other cells from hydrogen, Iron oxide,... some other noob things)... But I never really understood what to do...

Alan Yates likes to confuse the hell out of people by calling water an electrolyte (even though it is, but cmon it 's just water) and using weird chemicals :D

#55 Tweetybird88

Tweetybird88

    Pyromaniac

  • Full Member
  • PipPipPip
  • 151 posts
  • Location:USA
  • Interests:Fishing, hunting, pyrotechnics, chemistry

Posted 23 September 2007 - 10:12 AM

Yes. Titanium is cheap, I picked up a large sheet for $10. Lead dioxide will make the best anode.

Best anode for chlorate or best anode for perchlorate and chlorate. I hear platinum is better for perchlorate since it doesn't corrode hardl and it is a tad more efficient.

#56 frogy

frogy

    Pyrotechnician

  • Full Member
  • PipPipPipPip
  • 360 posts
  • Location:Kent, Ohio
  • Interests:Pyro, gaming, computers in general, paintball, potato guns...

Posted 23 September 2007 - 10:42 AM

Platinum\Iridium is good for perchlorate.. I'm now sure how good it is for chlorate though...

Graphite\Titanium supposably work for chlorate, but I believe both corrode\erode (graphite definitely does)...

I can get titanium sheet\rod stock very cheap at some local hardware stores... but I don't really know where to get platinum wire...

I have saw some platinum\Ir anodes on ebay though they're not there at the moment...

#57 hashashan

hashashan

    Pyromaniac

  • Full Member
  • PipPipPip
  • 164 posts

Posted 23 September 2007 - 12:47 PM

Titanium is crap. It will passivate within minutes and become useless as anode, however it will make a great cathode.
Platinum is good if you keep the chloride levels high when making chlorate and chlorate levels high for perchlorate. If you'll try to go straight Cl->ClO4 you will kill your anode eventually.
Lead dioxide is perfect for direct Cl->ClO4

YOU CANT MAKE PERCHLORATE FROM K-CHLORATE. It is just not soluble enough for any normal yield. You have to use a soluble chlorate like Lithium, Barium, Strontium, Sodium but never Potassium.
  • tortoise likes this

#58 Mumbles

Mumbles

    Grandmaster

  • Admin
  • PipPipPipPipPipPipPipPipPipPip
  • 11,776 posts
  • Gender:Male
  • Location:Above You

Posted 23 September 2007 - 01:41 PM

It's almost painful reading this thread.

Unless you're in france, I believe you will have trouble finding sodium chlorate as a herbicide.

KCl is not water softener salt. It is available as a water softening salt, but is much rarer than the sodium variety. I believe it is in a purple or green bag, and runs about $7-8 a 55lb bag. It is also available as Muriate of Potash in garden centers. "Lo-salt" and other low sodium salts are often a mix of NaCl and KCl.

Graphite is the standard electrode material for chloride to chlorate. It is cheap and readily available. It will start to corrode at low chloride concentrations however. I believe it is standard practice to run to 10-15% chloride, and remove the chlorate.

Lead Dioxide and platinum are the standard materials for chlorate to perchlorate. Platinum will corrode very fast if you try to go direct from chloride to perchlorate. The Lead Dioxide might be able to handle it. For purity and longevity of the anode purposes, it is often advisable to purify the chlorate from chloride before attempting to convert it to perchlorate.

To prepare potassium chlorate from the mother liquor of NaClO3 and NaCl you boil it, filter any insolubles, like graphite, and add a saturated soln of KCl. You then cool it to near freezing. The KClO3 will precipitate out. One to two more recrystalizations is advisable to get a pure product.

That method given by Hashashan for conversion of K Chlorate to Na Chlorate is rediculous. There is no reason for a reconversion to sodium. Secondly, adding the ethanol will just precipitate a variety, and leave you with a cocktail of various compounds. To get pure enough chlorate for perchlorate, filter any insolubles, boil the mother liquor until crystals just start to appear, and cool to near freezing again. NaCl solubility changes very little over the temperature range, so very little will precipitate. A second recrystalization will yield a product pure enough for perchlorate conversion.

You can make Potassium Perchlorate from Potassium Chlorate, just not by way of electrolysis very well.
  • tortoise and Sulphurstan like this
Just so you guys quit asking, here is the link to the old forum. http://www.xsorbit2....forum/index.cgi

The sky is my canvas, and I have 2,113 pounds of powdered paint in the workshop.

#59 WarezWally

WarezWally

    Pyrotechnician

  • Donator
  • PipPipPipPip
  • 701 posts
  • Location:The land down under

Posted 23 September 2007 - 03:12 PM

Best of luck to those trying to find suitable anodes for perchlorate production. If you have 70%+ nitric acid you can try making your own GSLD or TSLD anode which if well made should last quite a while.

#60 hashashan

hashashan

    Pyromaniac

  • Full Member
  • PipPipPip
  • 164 posts

Posted 23 September 2007 - 03:22 PM

Mumbles you are entering my specialty here :)
However if you do insist to go into a debate I'll translate a part of the book where i read it and DID IT.

here we go :
Dissolve 100 grams of KClO3 and 60 grams of Na2SO4 in 600 ml of water. While hot add 375ml of EtOH(K-sulfate will immediately precipitate), leave the vessel to stand for 2 days. decant the fluid and save it. Wash the K-sulfate with 30% EtOH and save the liquid. Pour the two liquids in one vessel and distill off the EtOH(if you need it).
Boil the liquid until crystals start to form, cool and filter. For a more pure product recrystallize from water.

Sorry for my bad translation I really don't have the nerves to rephrase it :)\

And about making KClO4 from KClO3 being impossible i meant electrolysis. Of course there are other working method.




1 user(s) are reading this topic

0 members, 1 guests, 0 anonymous users