Purification of sodium chlorate (removal of sodium chloride)

Purification of sodium chlorate (removal of sodium chloride)

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?

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

NaClO4 from NaClO3 via acetone

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.......LL
Ratios are on 100 gram of crude NaClO4 + 300g acetone. MAximal dissolving takes about 24 Hrs at 25 C.

Quote: Originally posted by Simoski

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

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/

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

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]

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]

Quote: Originally posted by Simoski

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

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.......LL

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.........LL

Quote: Originally posted by mysteriusbhoice

I have a very effective method to do this but it is rather long. you can use an ultrasonic humidifier or a simple humidifier and aquarium air pump to pump humid air to mixture of NaClO3 and NaCl the chlorate will dissolve leaving the NaCl undissolved. you want to occasionally remove any free liquid to expose more salt and to allow better diffusion into the solid. a temperature difference also helps where air pump + NaClO3 mix is in a colder room or the humidifier is hot. repeat till no more standing liquid forms and the remaining salt is NaCl. the liquid will be pure NaClO3 solution with very little NaCl which is not hygroscopic then you can simply boil down the liquid and filter the salt.

Quote: Originally posted by caterpillar

Quote: Originally posted by mysteriusbhoice   I have a very effective method to do this but it is rather long. you can use an ultrasonic humidifier or a simple humidifier and aquarium air pump to pump humid air to mixture of NaClO3 and NaCl the chlorate will dissolve leaving the NaCl undissolved. you want to occasionally remove any free liquid to expose more salt and to allow better diffusion into the solid. a temperature difference also helps where air pump + NaClO3 mix is in a colder room or the humidifier is hot. repeat till no more standing liquid forms and the remaining salt is NaCl. the liquid will be pure NaClO3 solution with very little NaCl which is not hygroscopic then you can simply boil down the liquid and filter the salt. maybe water steam will work faster?

I have a picture of my chlorate recovery tower.
I use it after fractional crystalization to pull out any remaining chlorate.
If you live in a country with high humidity and temperature then this setup will be faster.
You can also use a humidifier + demister(sponge) to put hot humid air though the setup ensuring temperature stays constant to prevent condensation from forming which could cause NaCl to dissolve.
using that setup you can lazily just evaporate your cell contents and plock it all in a large version of this and play the waiting game while you do other things.
this is from my old dirty batches with chromates and all this will be precipitated out using potassium salt.
If you use chromates either remove them first or dont use them and instead just use CaCl2 pH control in your run since it wont contaminate your batch and works better as an additive to your cell anyway.



[Edited on 8-7-2020 by mysteriusbhoice]