making potassium (per) chlorate

[taiwanluthiers]

Epoxy wouldn't hold up to cell conditions... in my cell I used epoxy to seal the connections, it works to a point but the epoxy would degrade eventually, even more so when used as an anode.

[schroedinger]

Even it won`t work with the normal MnO2 from batteries. It`s quite dirty crap.

 

The way you should go is to produce /buy highly purrified MnO2, use Nitric acid to make Manganese Nitrate.

Get the solution apart from the left over MnO2.

Evaporate you solution until it starts to crystallise (if to much crystallises, add dest aqua).

Paint solution onto Titanium (very thin) and Heat on a heating plate to 300°C+, repeat until you got a nice layer.

 

You will find both things on Nurd-Range (Youtube, Purifing MnO2 and plating it on to Titanium).

 

But to make it easy, i would recommend, making Manganese Nitrate straigt from Manganese Metall and Nitric acid, with Hydrogen Peroxide (Needed to save nitric acid, as Manganese need to be oxidised. Using HNO3 for that would be a waste).

 

Actually I`m also working on Plating it by electrolysis,but will take some time to make this work out

[THEONE]

I can not find here anywhere any of acids except hydrochloric but is maybe be 5-10% solution.

 

When you have any news about plating with electrolysis let us know how it works

[pdfbq]

Nurdrage did not manage to get a sustainable anode, neither did I. You get nice colors though

[schroedinger]

There are to vids on Nurdrange, the first on is made with the MnO2 from batteries, and its crap. Then there`s a second one, which is made from the purrified stuff with he stattes that it holds up god, if used with low current density.

 

When i tested my first one, it worked quite god. But still would to do it by electrolysis, to get a nice and thick layer.

 

Also there is a different way an Sciensmadness for a MMO anode, based on SnO2, dopped with antimony and lead, plated onto Aluminium. I never managed to make one of those. As i can't get the right soldering tin. Making it straight from Antimony an Sn Metall and Nitric acid, didn't work out, as it allways peeled off when getting heated

[THEONE]

out of sodium chlorate-perchlorate solution, that has been done by electrolysis of table salt, how we can calculate the amount-mass of potassium- ammonium nitrate to make potassium - ammonium perchlorate and potassium chlorate ??

[schroedinger]

Where`s the probem?

 

First step needs to be that you take harvest the Sodium perchorate and purify it. Then you got it as Crystalls, and go the normal way.

 

Never go straight from cell liquer to your product, as you allways will get problems with chlorates and some other things still in your cell.

 

Won't immagine what could happen if you think it's Pottasium perchlorate, mix it with Sulfur or wors`t case got a mix out of Ammonia Perchlorate and Chlorate. In that case you can probably say that you won`t see your building place again

Edited February 21, 2013 by schroedinger

[THEONE]

Where`s the probem?

 

First step needs to be that you take harvest the Sodium perchorate and purify it. Then you got it as Crystalls, and go the normal way.

 

Never go straight from cell liquer to your product, as you allways will get problems with chlorates and some other things still in your cell.

 

Won't immagine what could happen if you think it's Pottasium perchlorate, mix it with Sulfur or wors`t case got a mix out of Ammonia Perchlorate and Chlorate. In that case you can probably say that you won`t see your building place again

 

What are the steps you need to follow to purify your NACLO4/NACLO3 and prepare it for KCLO4/KCLO3 or NH4CLO4 ?

 

Also i have notice that it is better to make KCLO4 or NH4CLO4 with nitrates cause NANO3 is much more soluble than NACL correct ?

Edited February 21, 2013 by THEONE

[taiwanluthiers]

If you have chlorate in your potassium perchlorate, you can chemically destroy it then purify them. For Ammonium perchlorate you must do this before the conversion... however I am not sure if you want to make AP from sodium perchlorate, because you won't get the sodium out...

 

Swede has a blog entry on this...

[schroedinger]

First stepp will be destroing hypochlorite by boiling.

Next filter solution.

Then destroy Chlorate, there are different way`s, just look em all up in the oocities blog.

But probably first by decomposing by heat, and then destroy by use of hydrochloric acid.

Next would be testing that you`ve really destroyed all chlorate (for example methylenblue).!!!!!!!!!!!!!!!!!!

If you wan`t you can now measure your leftover amount of chloride.

Now make what ever Salt you want to make.

 

 

 

By the way, i`ve got a question regarding towards pottasium perch. Most sources you read that`s impossible to make KClO4 from KCl, but other say, just keep the cell warm and it works. Which one is right?

[THEONE]

If you have chlorate in your potassium perchlorate, you can chemically destroy it then purify them. For Ammonium perchlorate you must do this before the conversion... however I am not sure if you want to make AP from sodium perchlorate, because you won't get the sodium out...

 

Swede has a blog entry on this...

 

By adding a solution of ammonium nitrate (not ammonium chloride!!) in correct quantities into a solution of sodium perchlorate you will take ammonium perchlorate and sodium nitrate, were sodium nitrate is much much more soluble in water than ammonium perchlorate!!

 

http://www.oocities.org/capecanaveral/campus/5361/chlorate/ammper2.html

Edited February 21, 2013 by THEONE

[Mumbles]

Both are right in a way. It is chemically and physically possible to make potassium perchlorate starting from potassium chloride. However, due to the relatively poor solubility of potassium chlorate it is not an economical or commercially viable route. It's physically possible, but has significant disadvantages. For small scale hobby setups, I believe it's been shown to not be that big of a deal. The batch sizes are still good enough for us.

 

...

 

By the way, i`ve got a question regarding towards pottasium perch. Most sources you read that`s impossible to make KClO4 from KCl, but other say, just keep the cell warm and it works. Which one is right?

[schroedinger]

Ok, thx, that could make some things much easier, if thinking of sodium

[pdfbq]

First stepp will be destroing hypochlorite by boiling.

Next filter solution.

Then destroy Chlorate, there are different way`s, just look em all up in the oocities blog.

But probably first by decomposing by heat, and then destroy by use of hydrochloric acid.

Next would be testing that you`ve really destroyed all chlorate (for example methylenblue).!!!!!!!!!!!!!!!!!!

I don't think there is much hypochlorite left in a perchlorate cell.

Filter, yes you can, but i would filter later.

Decompose chlorate by heat? That's at ~350C iirc so you first have to get rid of all the water and its pointless anyway.

HCl is dirty. I use sodium metabisulphite. Easy, cheap and 100% effective.

Methyleneblue test for perchlorate. You need indigo carmine to test for chlorate.

 

 

@THEONE

Why not Ammonium chloride? Works fine is my experience.

 

@taiwanhunters

Yes you can get the sodium out but you loose quite a bit. One way to cope with that is convert your dirty leftover Aperc/NaCl solution to Kperc.

Edited February 22, 2013 by pdfbq

[THEONE]

@THEONE

Why not Ammonium chloride? Works fine is my experience.

 

Cause sodium nitrate (730gr/L solubility at 0°C) has a much more solubility in water than ammonium chloride (297gr/L solubility at 0°C)

[schroedinger]

Yes you would need 350°C for decomposing chlorate to perc.

But your right, there are some different ways for destroying perc which way you chose allways depends mainly on your abbilities.

 

If hypochlorite is still in your cell, depends allways on the way you made the perc, eg. if youre where gone straight from chloride, you should make sure to destroy it.

Even if you where going from chlorate, still would make sure that all of it is destoyed, as it will be inside.

I'm not sure if Aceton can react with perc/chlorate in aqua solution, but if not, would be perfect. As you could add that to, to form chloroform. Couldn't find any informations about that, looks more like they won't react.

 

Test for chlorate is indigo carmine, for perc is methylenblue, thats right.

 

.

[THEONE]

Before 2 days i started with a cell of about 1L solution of nacl

I run it with a voltage of 5 volts and about 1.5A.

After 2 days i remove the set-up and i boiled down the solution for 15 minutes. Then i ad to this solution a solution of kno3 (cause i did not have kcl) and in the end i didn't take nothing, but anyway i am steel at the beginning.

 

NOTES.

1 ) When the cell was running a strong smell of chlorine comes out.

2) I didn't use something to watch the temperature - pH and the electrolyte (cause it was outside) may had a temperature of 10-20°C

3) The anode was 5 graphite rods from some carbon-zinc batteries and cathode stainless steel

4) The solution after some amount of time turned to yellow and at the bottom has some yellow - black material, so i filter it out. After that it had a yellow colour.

5) After filtering the electrolyte, i boil it and after it starts to boil, from a yellow colour, starts to became a very deep black colour so i filter it again when the boiling processes ends. A yellow colour electrolyte again come to place

6) Then i add a hot solution of kno3 to the electrolyte and i let it cool outside (5-10°C)

7) As i say before, i didn't get anything.

Edited February 23, 2013 by THEONE

[taiwanluthiers]

How big was the cell? I converted about 500g of potassium chlorate running at around 10-15 amps a week, with a 2 liter cell. If you are running at 1.5 amps then you need more than just a few days.

[THEONE]

How big was the cell? I converted about 500g of potassium chlorate running at around 10-15 amps a week, with a 2 liter cell. If you are running at 1.5 amps then you need more than just a few days.

 

It was plastic bowl full of 1L of nacl solution

[taiwanluthiers]

The cell should be sealed too, otherwise everything around the cell will corrode due to salt spray.

 

Also how concentrated was the solution? They should be nearly saturated... low chloride level kills anodes. You should get MMO anodes if you get the chance, they are cheap and does not corrode like graphite.

Edited February 23, 2013 by taiwanluthiers

[THEONE]

The cell should be sealed too, otherwise everything around the cell will corrode due to salt spray.

 

Also how concentrated was the solution? They should be nearly saturated... low chloride level kills anodes. You should get MMO anodes if you get the chance, they are cheap and does not corrode like graphite.

 

PVC cell will work well ??

[schroedinger]

PVC is a chlorinated plastic, which hold up quite god to a cell.

 

But like it`s said above, you probably didn`t form much of a chlorate, as 1.5 amps at 48 hours will just be able to convert 19,59 grams of chloride into chlorate. but thats at 100% ce. With that setup you maybe got 8-10 gramms converted. so you can test for chlorate, and will find some. But you just produced enought, that everything is still dissolved.

 

Also don`t operate a chlorate cell at 10-20°C, thats to cold. Depending on your Anode run it between 40-60°C

[THEONE]

Also something else. Cause i did not have an easy access on kcl - nh4cl i am going to use kno3 and nh4no3.

So 100gr of saturated solution of NACL how much amount of kno3 -nh4no3 must add to make kclo3-kclo4-nh4clo4 ?

Edited February 23, 2013 by THEONE

[pdfbq]

You do not add anything to your NaCl cell until you run it.

Please do not add any NH4NO3 to your cell befor you exactly know what you are doing.

Ammonium Nitrate together with chlorate is as far as I know asking for big trouble.

 

But to give an answer to your question. You can calculate the amounts by writing down the displacement reactions and then

look up the molar mass of the molecules.

[THEONE]

You do not add anything to your NaCl cell until you run it.

Please do not add any NH4NO3 to your cell befor you exactly know what you are doing.

Ammonium Nitrate together with chlorate is as far as I know asking for big trouble.

 

In case of kcl - nh4cl i am going to use kno3 -nh4no3 for metathesis reaction, i am not planning to add anything on it when it is running

 

You can calculate the amounts by writing down the displacement reactions and then

look up the molar mass of the molecules.

 

Can you give me an example, for lets say nacl-->(electrolysis)naclo3--> (kno3 metathesis) kclo3

Edited February 23, 2013 by THEONE