Sciencemadness Discussion Board

Purification of sodium chlorate (removal of sodium chloride)

Simoski - 1-4-2019 at 03:56

Hi I have created a significant amount of sodium chlorate and want to purify it to the point where the sodium chloride present will not negatively effect my platinum plated titanium substrate anode when I use it to create perchlorate .

Does anyone have any tips for separating chloride from chlorate?

Are there any inorganics that will selectively react with chloride and not chlorate?

I keep thinking multiple recrystalisations but it seems so tedious and time consuming, surely there is a simpler route?

Ubya - 1-4-2019 at 04:14

you can remove chlorides ions with silver nitrate, but the you would have nitrate ions in solution and i don't know if they would interfere

Purification of sodium chlorate (removal of sodium chloride)

Simoski - 1-4-2019 at 09:50

Hi I have created a significant amount of sodium chlorate and want to purify it to the point where the sodium chloride present will not negatively effect my platinum plated titanium substrate anode when I use it to create perchlorate .

Does anyone have any tips for separating chloride from chlorate?

Are there any inorganics that will selectively react with chloride and not chlorate?

I keep thinking multiple recrystalisations but it seems so tedious and time consuming, surely there is a simpler route?

fusso - 1-4-2019 at 09:53

Why're you double posting?

Simoski - 1-4-2019 at 09:56

Sorry I am not sure how I did that, it was a mistake

Laboratory of Liptakov - 1-4-2019 at 12:30

How to obtain NaClO4 from NaClO3 without platinum (or else anode) via acetone process, during a few hours:
https://www.youtube.com/watch?v=1Ylt2ZKJlME

markx - 2-4-2019 at 01:42

Quote: Originally posted by Simoski  
Hi I have created a significant amount of sodium chlorate and want to purify it to the point where the sodium chloride present will not negatively effect my platinum plated titanium substrate anode when I use it to create perchlorate .

Does anyone have any tips for separating chloride from chlorate?

Are there any inorganics that will selectively react with chloride and not chlorate?

I keep thinking multiple recrystalisations but it seems so tedious and time consuming, surely there is a simpler route?


There will always be an equilibrium of chloride that develops in a perchlorate cell, even when pure chlorate is used as the starting material. It develops due to cathodic reduction of the chlorate ions and also due to certain side reactions.

Those in command of the german language might find the attached information useful:

Attachment: Chlorate und Perchlorate.pdf (2.2MB)
This file has been downloaded 79 times

morganbw - 2-4-2019 at 14:49

Quote: Originally posted by Laboratory of Liptakov  
How to obtain NaClO4 from NaClO3 without platinum (or else anode) via acetone process, during a few hours:
https://www.youtube.com/watch?v=1Ylt2ZKJlME


Not viewed yet but did subscribe. Will watch soon, thank you.

NaClO4 from NaClO3 via acetone

Laboratory of Liptakov - 3-4-2019 at 04:56

Markx have right. During process from NaClO3 on NaClO4 arises next compounds, which can damage Platinum surface. Next way is use PbO2, which is resistant against NaCl in solution. Is resistant agains anythig compounds during proces. But problem can be original factory quality of this PbO2 anodes. Which go on sale around the world. Therefore I am prefer method heating NaClO3 (+ NaCl residuum) from chlorate cell, heating process on 500 C and forming NaClO4 + NaCl (+ NaClO3 residuum). In acetone are dissolve only NaClO4. All others compounds remain as powder on the bottom of glass jar....:cool:...LL
Ratios are on 100 gram of crude NaClO4 + 300g acetone. MAximal dissolving takes about 24 Hrs at 25 C.

Simoski - 3-4-2019 at 12:26

So it looks like I have to live with the chloride erosion. Thank you gentlemen.

j_sum1 - 3-4-2019 at 15:23

Merged with duplicate thread. Sorry if this tangles the discussion a bit.

markx - 3-4-2019 at 23:27

Quote: Originally posted by Simoski  
So it looks like I have to live with the chloride erosion. Thank you gentlemen.


You have to look at your Pt plated anode as a consumable item when engaging in perchlorate synthesis. There really is no good way around it I'm afraid. Most of the damage seems to happen at the end stages of the conversion, so if one stops before chlorate becomes badly depleted from the cell, then a lot more life can be squeezed out the anode.
Then an acetone based separation can be done on the mix, to yield a pure product. Or one can go the thermal decomposition route from the chlorate and omit the electrosynthesis stage. I would suggest to rig up a PID controlled heating setup for the purpose and make sure one has no organic or metallic contaminants in the chlorate stock. A lot of metal salts are catalysts for the thermal chlorate decomposition and steer the reaction towards evolution of oxygen and chloride. Notably iron and manganese compounds. Thus a properly contaminated batch can yield no perchlorate as a result or the yield shall suffer badly. But it is a quick and relatively simple method that can process rather large quantities in a short time. At least compared to electrolysis.

yobbo II - 6-4-2019 at 14:05

Take out solid sodium chlorate from the cell by running long enough (and adding more salt to convert to chlorate) so that the Na chlorate starts to deposit on the cell bottom. Give it a single wash in ice water and it will be OK for going onto perchlorate with a Pt anode.

https://geocitieschloratesite.000webhostapp.com/

Simoski - 8-4-2019 at 11:24

Quote: Originally posted by yobbo II  
Take out solid sodium chlorate from the cell by running long enough (and adding more salt to convert to chlorate) so that the Na chlorate starts to deposit on the cell bottom. Give it a single wash in ice water and it will be OK for going onto perchlorate with a Pt anode.

https://geocitieschloratesite.000webhostapp.com/


Ok fantastic, I vacuum filtered it, then recystalised it.... so I feel good to push for the perchlorate

[Edited on 8-4-2019 by Simoski]

Simoski - 8-4-2019 at 11:31

Quote: Originally posted by Ubya  
you can remove chlorides ions with silver nitrate, but the you would have nitrate ions in solution and i don't know if they would interfere


I really like this idea, now all we need is a way to remove the nitrate ions! Ideas please gentlemen....

Would copper nitrate do the same... yield CuCl2 and drop out leaving the nitrate ion behind in solution??

[Edited on 8-4-2019 by Simoski]

MrHomeScientist - 8-4-2019 at 12:47

Look up the solubility for any proposed substitues: copper chloride is soluble, while silver chloride is not. That's why silver works.

markx - 9-4-2019 at 06:26

Quote: Originally posted by Simoski  


I really like this idea, now all we need is a way to remove the nitrate ions! Ideas please gentlemen....

Would copper nitrate do the same... yield CuCl2 and drop out leaving the nitrate ion behind in solution??

[Edited on 8-4-2019 by Simoski]


There is really very little point in trying to remove the last bit of chloride from the chlorate stock prior to perchlorate synthesis. In all probability one shall introduce more contaminants into the stock by the process and gain nothing in return. Some of the contaminants may have deleterious effects upon later perchlorate conversion.
Excess chloride shall be converted to chlorate at the Pt and the equilibrium concentration is there anyways, so not to worry.
As far as I've seen from my experience, the initial stages of perchlorate synthesis shall hardly cause damage to the platinum. It is the end phase where chlorate depletion steps in that seems to munch away on the Pt at a nice rate. And I've never used purified NaClO3 for the purpose....just plain solution straight from the chlorate synth stage. It definitely contains some excess chloride to begin with.

In fact I read a patent regarding the Pt erosion in perchlorate cells and it was stated that Pt erosion can be held at a minimum if a certain ratio of ClO3- /ClO4- is maintained in the cell. It seemed quite cumbersome and challenging to monitor and maintain this ratio, so I did not spend too much attention to the document. I'll try to find the reference....

Found it:



[Edited on 10-4-2019 by markx]

Attachment: US3475301.pdf (772kB)
This file has been downloaded 56 times


Simoski - 11-4-2019 at 05:10

Quote: Originally posted by markx  
Quote: Originally posted by Simoski  


I really like this idea, now all we need is a way to remove the nitrate ions! Ideas please gentlemen....

Would copper nitrate do the same... yield CuCl2 and drop out leaving the nitrate ion behind in solution??

[Edited on 8-4-2019 by Simoski]


There is really very little point in trying to remove the last bit of chloride from the chlorate stock prior to perchlorate synthesis. In all probability one shall introduce more contaminants into the stock by the process and gain nothing in return. Some of the contaminants may have deleterious effects upon later perchlorate conversion.
Excess chloride shall be converted to chlorate at the Pt and the equilibrium concentration is there anyways, so not to worry.
As far as I've seen from my experience, the initial stages of perchlorate synthesis shall hardly cause damage to the platinum. It is the end phase where chlorate depletion steps in that seems to munch away on the Pt at a nice rate. And I've never used purified NaClO3 for the purpose....just plain solution straight from the chlorate synth stage. It definitely contains some excess chloride to begin with.

In fact I read a patent regarding the Pt erosion in perchlorate cells and it was stated that Pt erosion can be held at a minimum if a certain ratio of ClO3- /ClO4- is maintained in the cell. It seemed quite cumbersome and challenging to monitor and maintain this ratio, so I did not spend too much attention to the document. I'll try to find the reference....

Found it:



[Edited on 10-4-2019 by markx]


Thank you very much Markx.

Will I increase my yield using a clay pot as a diaphragm ?

markx - 11-4-2019 at 08:55

Quote: Originally posted by Simoski  



Will I increase my yield using a clay pot as a diaphragm ?


I do not think so....unless you try to produce HClO4 in the anode compartment I see no real point in using a membrane cell. Legend tells that a separated cell enables one to produce perchlorate on graphite anode, but I highly doubt that it will accomplish anything more than a mere partial separation of anodic and cathodic products.

JohnDoe13 - 16-4-2019 at 04:52

https://www.youtube.com/watch?v=r7R_LRgN3f0

yobbo II - 29-4-2019 at 11:17

Pt erosion is a serious problem if you are using Pt plated (as opposed to clad or solid) anodes. The plated stuff is not as erosion resistant as clad/solid and can only be applied as a very thin coating. No one here has clad anodes that I know of, they would be a professional job only and very expensive, IMO. Get solid anodes by beating/rolling out bullion or perhaps wire. These are quite resistant to residual amounts of chloride.

The divided perchlorate cell patent is a very old patent and is nonsense to boot.

Yob

Laboratory of Liptakov - 29-4-2019 at 13:49

yobbo II ....Has Truth. Pt anode coated film type, is loss of money and time. Thus for most amateurs. Maybe someone has good results, but watching ratios compounds in solution is mad work. How say again, methode NaClO3 (with impurities) =heating= NaClO4/NaCl=acetone= NaClO4 provide good purity for using on EM field. And mainly is it quick. During a few hours. And not need wait for 3 days, how is concentration NaClO4 in solution. Anyway, there will be a few percent of NaClO3. As with the acetone method.

Laboratory of Liptakov - 10-5-2019 at 00:35

Here is example uncomplete reaction at 500 C. In glass you an see 2 layers. Down is NaCl, up is NaClO3, in acetone is NaClO4. His solubility is 52g in 100g of acetone. Solubility others is zero grams on 100g of acetone....:cool:...LL

NaP.JPG - 971kB

Gargamel - 13-5-2019 at 08:30

Your acetone method looks interesting Doc.

But as acetone is a known precursor for EM I would not dare to buy this in larger quantity from chemistry shops.

Only hardware/paint store stuff can still be had anonymous.
Any idea to clean this up effeciently some way but destilling it?
I prefer not to destilll such flammable stuff.

Laboratory of Liptakov - 13-5-2019 at 12:05

Almost all is precursor in today times. EM or drugs. A lot chemicals is impossible get without adress. Dont worry, be happy. Distillation acetone is normal easy process. Water bath 90C = cooler= ice bath zero C. Tested, confirmed. Is it even without smell on output side. Thanks ice bath. Most worst is the death from fright and from fear.....:cool:....LL