making potassium (per) chlorate

[THEONE]

Ok so here is what i found.

 

nacl have 58.44 g/mol

naclo3 have 106.441 g/mol (nacl-->naclo3 106.44/58.44=1,82)

kno3 have 101.1032 g/mol (101.1032/106.441=0,9498)

kclo3 have 122.5495 g/mol (122.5495/106.441= 1,15)

 

So for 100gr of nacl you will have 182gr of naclo3

And to turn it to kclo3 you will need 182*0,9498= 172,8gr of kno3

And you will have 182*1,15=209,3 gr of Kclo3 correct ?

[pdfbq]

Yes, looks OK to me.

 

The problem though is that you can not run your cell till all NaCl has become NaClO3.

I still do not know how to handle that but an idea is to crystallize the NaClO3 out and dry.

 

Making KClO4 is less difficult. I just add enough KCl to a NaClO4 solution until nothing drops out anymore (and add a little more, just to be sure).

Edited February 24, 2013 by pdfbq

[schroedinger]

Yes your way of preparation looks fine to me. But be aware, like said, you cant convert all Chloride.

And you won`t make ´106,44 g NaClO3 from 58,44 g NaCl, as you will allways lose some amounts to NaOH and Cl2

 

Also, don`t try any Ammonia perc, if you don`t have loot of experience. I never did them, and won`t try it for a long long time, as it is just risky like hell, if your not 100% sure.

 

Even if I`m sure, i won`t do as i don`t need it

Edited February 24, 2013 by schroedinger

[THEONE]

Yes your way of preparation looks fine to me. But be aware, like said, you cant convert all Chloride.

And you won`t make ´106,44 g NaClO3 from 58,44 g NaCl, as you will allways lose some amounts to NaOH and Cl2

 

Also, don`t try any Ammonia perc, if you don`t have loot of experience. I never did them, and won`t try it for a long long time, as it is just risky like hell, if your not 100% sure.

 

Even if I`m sure, i won`t do as i don`t need it

 

I belive that we can very economically make some ammoniun perchlorate by this way out of table salt and ammonium nitrate

We must just to find a way to destroy any sodium chlorate into the electrolite and test it to be sure that there is no any chlorate inside

Edited March 1, 2013 by THEONE

[nemiisis]

For some reason i can't make a thread, i was wondering, I have a cell that is working kind of...

Graphite Electrode, Stainless steal cathode, Saturated potassium chloride solution.

However i will leave it on (5V, 26A) for 10-12 hours and absolutely nothing will crystallize.

Theres approximately 1L of Water.

[nemiisis]

For some reason i can't make a thread, i was wondering, I have a cell that is working kind of...

Graphite Electrode, Stainless steal cathode, Saturated potassium chloride solution.

However i will leave it on (5V, 26A) for 10-12 hours and absolutely nothing will crystallize.

Theres approximately 1L of Water.

 

Haha, i figured it out, my solution wasn't saturated enough.

[taiwanluthiers]

You also need more than 10-12 hours...

[nemiisis]

You also need more than 10-12 hours...

 

I'm making only chlorates, what i posted before is actually still not solved... i'm not sure what to do anymore.

[taiwanluthiers]

I used MMO and it took a week before the run is completed. I doubt anything will crystalize in 12 hours. I suggest MMO if you can get it, you won't end up with a bunch of graphite suspension.

[schroedinger]

No worries, the graphit shouldn`tbe a problem, Just hot filter youre solution and rinse the filter again with hot watter, and you`re fine.

 

But looking at your cell dates, there`s nothing to wonder about, 1L @ 26 amps, you will get a very hot cell (Probably around 80°C to boiling) and at this Temperatures KClO4 won`t cristallyse, as it is in solution

[taiwanluthiers]

Just beware that cell liquor can actually dissolve filter paper a bit... don't ask how I know.

[nemiisis]

So now it appears my power supply is completely broken.

I connect the green and black wires like normal, then put my red and black wires on my cell, and it doesn't turn on.... =/

 

Got a new power supply (this one seems to work a bit better.)

Only problem is i don't know which wire is what Volt / Amps

 

I'll update when i see crystals (This cell doesn't get hot at all, standard room temp)

Edited March 3, 2013 by nemiisis

[schroedinger]

That sounds like youre using an ATX computer power supply. With these aways connect green to Black for start.

 

Then connect red and black towards cell.

 

After that put a ressistor into the 12V line (yellow to black) or something that works like a Ressistor (e.g. connect an Old Harddrive). If you just connect the 5V line, you will ruin your power supply. This is because of the way how these power supplies are constructed

[WSM]

I'm making only chlorates, what i posted before is actually still not solved... i'm not sure what to do anymore.

 

The typical chlorate cell will drop out very few crystals on the first run. Most of the energy is spent turning salt water into the precursers (hypochlorite, hypochlorous and chlorate species). Now after the first run, if you add fresh salt solution (I usually run KCl, by the way), the cell will very quickly start to produce chlorate crystals.

 

For the highest efficiency of a batch system, track the current (amps) going into the cell from the power supply. When the current drops to about half the peak current observed, stop the run, add more saturated salt solution (after harvesting the chlorate crystals), and run the cell some more. The reason we stop at the 50% current point is the cell uses MUCH more current past this point with very little increase in chlorate production (AND it's very hard on the electrodes, even MMO and titanium). It's been called "diminishing returns" and it's real.

 

If you're running sodium chloride, I can't advise you. I haven't run NaCl in a cell yet. I'm sure I will at some point, but I'm not there yet. When we progress to the conversion of chlorate to perchlorate, the removal of residual chlorate (from the perchlorate solution) is usually done with SO₂ which can be generated by sodium or potassium metabisulfite solution. You can read Swede's blogs to see how he worked out the process (his first attempts were a bit wasteful, but he got better as he progressed).

 

Have fun and don't give up. You'll get there...

 

WSM

[nemiisis]

Only one question now, i've got everything setup, working perfectly

I was just wondering if Chlorates are only formed when the solution is warm, or can it be cool (20'C)?

[WSM]

Only one question now, i've got everything setup, working perfectly

I was just wondering if Chlorates are only formed when the solution is warm, or can it be cool

 

Chlorates can be formed when the cell runs cool, but the efficiency suffers. A hot running cell uses more power but is more efficient.

 

WSM

[schroedinger]

As some people said that MnO2 anodes won`t last.

 

I`ve made one new Up, on Ti. Works perfect with KCl

The way i`ve done it was:

 

Mix Mn metal with HNO3 and H2O2

Take the solution and aply it thin onto a sheet of Ti.

Heat it on a Hotplate to 350°C

Shake dust of.

Rinse with H2O dest.

Set aside for 1 minute.

Repeat 5 times

Then heat with a gas torch.

Repeat 5 times (2x)

 

Leave aside for 1-2 Day`s. Now shake of all dust and use at max of 200mA cm²

[frank]

As some people said that MnO2 anodes won`t last.

 

I`ve made one new Up, on Ti. Works perfect with KCl

The way i`ve done it was:

 

Mix Mn metal with HNO3 an..............

....................

 

Leave aside for 1-2 Day`s. Now shake of all dust and use at max of 200mA cm²

 

They have said that MnO2 does not last long when making Perchlorate.

Typical mix up / confusion caused by thread title.

[WSM]

They have said that MnO2 does not last long when making Perchlorate.

Typical mix up / confusion caused by thread title.

 

So true. The bulk of the postings here refer to chlorate production, which is the first big challenge we overcome. The next logical step is converting some of that chlorate into perchlorate.

 

Some have said that the processes are so similar that the title (per)chlorates is appropriate and covers all the bases. I think it muddies the water a bit. I also feel that chlorate production and perchlorate production have enough distinct parameters, and unique peculiarities, that they deserve separate attention. It's not apples and oranges, but maybe more of tangerines and grapefruits.

.

My two cents...

 

WSM

[taiwanluthiers]

Chlorate production must be 1000x easier than perchlorate production. All you need is a ATX power supply, a plastic bucket and MMO as well as Ti plate. Not terribly expensive. But perchlorate requires either platinum, or lead dioxide. Pt is expensive but works, and it erodes even if the best care is taken... LD is cheap so who cares if it erodes a few milligrams at a time, but nobody sells them so it requires expensive and complicated setup to make yourself...

 

It really feels like the perchlorate thing is leaps more work than chlorate.

[schroedinger]

In fact the perchlorate cell is less work than a chlorate cell. It`s working fast.

The cells are setup in the same manner, but the conditions in a chlorate are much more harsh then in a perchlorate cell.

 

The big thing about both cells is that you first need to set em up. And a chlorate cell operates at much higher temperatures then a chlorate cell.

 

But you`re right making the Anode is the big step here.

Edited March 7, 2013 by schroedinger

[WSM]

In fact the perchlorate cell is less work than a chlorate cell. It`s working fast.

The cells are setup in the same manner, but the conditions in a chlorate are much more harsh then in a perchlorate cell.

The big thing about both cells is that you first need to set em up. And a chlorate cell operates at much higher temperatures then a chlorate cell.

But you`re right making the Anode is the big step here.

 

I think you meant "a perchlorate cell operates at much higher temperatures than a chlorate cell".

• Not only that but a higher voltage, typically
  
• Also, pH does not play a significant role in the perchlorate cell
  
• The cell function is purely anodic and not a bulk reaction, if I understand it correctly
  

The anode is and has been the greatest challenge to making perchlorate on an amateur or experimental scale. What's needed is an anode as simple or uncomplicated (and inexpensive plus durable) for perchlorate production as MMO is for chlorate production. It may be out there, but so far, it's not easily had. There's the promise of future developments and I hope they're quick in coming, but in the mean time we do the best we can with what we have at our disposal.

 

WSM

Edited March 8, 2013 by WSM

[taiwanluthiers]

It's like bandsaw blades, most manufacturer of bandsaw blades cater to professional sawmills, at least for blade used for resawing, so they only stock really wide blades that won't fit on bandsaws that hobbyist has, and therefore selection is kinda poor... I guess any industry that caters only to hobbyist aren't making any money.

 

So same goes for perchlorate cell production... industry uses platinum because they have a means of recovering them if they do erode, so they can use the same platinum over and over again, but I am guessing nobody wants to make a commercial LD anode because platinum already works and they aren't going to produce LD anodes just for a few hobbyist. MMO was used in saltwater chlorination devices, which is more widely used than people making chlorate with them. It just so happens that they work great for chlorates.

Edited March 8, 2013 by taiwanluthiers

[WSM]

It's like bandsaw blades, most manufacturer of bandsaw blades cater to professional sawmills, at least for blade used for resawing, so they only stock really wide blades that won't fit on bandsaws that hobbyist has, and therefore selection is kinda poor... I guess any industry that caters only to hobbyist aren't making any money.

So same goes for perchlorate cell production... industry uses platinum because they have a means of recovering them if they do erode, so they can use the same platinum over and over again, but I am guessing nobody wants to make a commercial LD anode because platinum already works and they aren't going to produce LD anodes just for a few hobbyist. MMO was used in saltwater chlorination devices, which is more widely used than people making chlorate with them. It just so happens that they work great for chlorates.

 

MMO is used for saltwater chlorination devices, but also many other uses:

• cathodic protection systems
  
• chlor-alkali industry
  
• electrodes for various electrochemical processes
  
• possible electro-winning of various metals and elements
  

Various formulations in MMO have different properties that make them suitable for many different purposes. It's our hope that one or more may prove to be useful for the conversion of chlorates to perchlorates in a properly prepared cell. The future is wide open and many things are yet to be discovered. I just hope it doesn't take fourty years for the technology to be as common place as MMO for chlorates is today.

 

WSM

[schroedinger]

Nope, i was saying the thing that i wrote.

A Chlorate cell needs to be operated at a higher then a Perchlorate cell. If you are operating a Perc cell at high temperatures, you`re doing something wrong (expet for the KClO3 --> KClO4 route). if the temperature raises in the perc cell, you will get a higher production of oxigen.

 

Also you don`t need a higher voltage for a perchlorate cell. (But there a some reasons why it could be interesting to do so, as you can be sure that you are pumping enought amps into the cell)

 

Also you`re wrong the reaction is not pure anodic, there is even a lot of bulk reaction, but this part really depends on the way you`ve build your cell (mostly Placing anodes and amperes/temperature). (In a chlorate cell)

 

For the bulk reaction you will need 6 electrons for the Anodic on 9.

 

In the Perchlorate cell you really just got anodic reaction.

 

Edited March 9, 2013 by schroedinger