Rainwater
National Hazard
Posts: 919
Registered: 22-12-2021
Member Is Offline
Mood: indisposition to activity
|
|
Cleaning potassium chlorate
I recently suffered from the purchase of fake titanium and its use in a simple potassium chlorate cell.
Platinum on titanium anode. Undamaged
Fake titanium cathode. Severely corroded.
And a beautiful pink electrolyte.
After decanting and 3 hot filterations and recrystallizations using dH2O. I'm left with these ugly crystals. And about 40% of my original yield
These brown follows both my solids and liquids
So a few googles about alloys and a few tests I'm showing Mn+2 ions in solution.
How i tested for Mn ions is as follows
adding NaOH solution, drop-wise, to a test tube containing the pink solution, a white precipitate formed and quickly (30s) turned brown.
After redoing the test with much less sodium hydroxide the precipitate stayed white until i bubbled air through it which left a pink solution with
brown precipitate.
.
Currently out of HCl solution but i want to try to convert the brown to a soluble state. MnCl2
Would small carefully added amounts of hcl be able to do this without destroying my desired product?
"You can't do that" - challenge accepted
|
|
|
MadHatter
International Hazard
Posts: 1339
Registered: 9-7-2004
Location: Maine
Member Is Offline
Mood: Enjoying retirement
|
|
Platinum/Titanium Anode
Manganese from the cathode ? That's weird. Your use of platinum sounds like
you're attempting to produce the perchlorate. I always used gouging(carbon) rods
for my cathode. Your cathode sounds like an alloy. As for adding HCl to your brine,
I wouldn't recommend it if chlorate is the desired product. Chlorate and HCl
react producing gas. Gas can be chlorine, hypochlorous acid or chlorine dioxide
depending on pH. When making the perchlorate via electrolysis leftover chlorate
is destroyed by HCl.
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
|
|
|
Rainwater
National Hazard
Posts: 919
Registered: 22-12-2021
Member Is Offline
Mood: indisposition to activity
|
|
Na I'm just aiming for chlorates.
So what I tried with a test tube is to bubble air through my solution with some nasty solids in it. This morning the pink was gone with a lot more
brown in my crystals. I then heated the solution with additional water until all that was left was a brown sludge. Filtered and obtained pure white
crystals. Now i just have to convert my full batch and hope the procedure scales up from the test tube to the kilogram i was hoping for. Getting ready
for the new years with some custom shower effects
Edit:
First batch looks great after vacuum drying
[Edited on 30-7-2022 by Rainwater]
"You can't do that" - challenge accepted
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
