Scorpion812 Posted September 19, 2017 Posted September 19, 2017 Hey everyone,So i am planning on building a chlorate and a perchlorate cell very soon, and i know that i will have to destroy chlorate from my KClO4. I am planning on doing the HCl/K2S2O5 or the HCl/FeSO4 approach. I know that there is gonna be ClO2 and Cl2 when I add the acid. Is this very dangerous?What tips do you have on destroying chlorate? does anyone have experience using the FeSO4 method as it isn't really documented very well on the chlorates site? What base should I use to neutralise? KOH? thanks in advance
Arthur Posted September 19, 2017 Posted September 19, 2017 If you start with sodium salts then the addition of KCl solution as final metathesis precipitates KPerc first then if you overdo it K chlorate drops out later. Best that you gradually add KCl and take the KPerc off carefully before the KChlorate drops out. This means that your K Perc is much purer to start with then only a little (if any) chlorate needs destroying meaning that very little of both noxious gasses produced will need venting. Careful fractional crystallisation is your best friend here. Also every bit of chlorate destroyed is chlorate that cannot be electrolysed later so destroying chlorate is also wasteful.
Scorpion812 Posted October 9, 2017 Author Posted October 9, 2017 If you start with sodium salts then the addition of KCl solution as final metathesis precipitates KPerc first then if you overdo it K chlorate drops out later. Best that you gradually add KCl and take the KPerc off carefully before the KChlorate drops out. This means that your K Perc is much purer to start with then only a little (if any) chlorate needs destroying meaning that very little of both noxious gasses produced will need venting. Careful fractional crystallisation is your best friend here. Also every bit of chlorate destroyed is chlorate that cannot be electrolysed later so destroying chlorate is also wasteful. I know that you have to add the KCl slowly, but if you use a chlorate destruction method that generates dangerous gases, is everything fine if you just stay outside?what do you if you get that nasty gas?
WSM Posted October 10, 2017 Posted October 10, 2017 (edited) Hey everyone,So i am planning on building a chlorate and a perchlorate cell very soon, and i know that i will have to destroy chlorate from my KClO4. I am planning on doing the HCl/K2S2O5 or the HCl/FeSO4 approach. I know that there is gonna be ClO2 and Cl2 when I add the acid. Is this very dangerous?What tips do you have on destroying chlorate? does anyone have experience using the FeSO4 method as it isn't really documented very well on the chlorates site? What base should I use to neutralise? KOH?thanks in advance I've used sodium metabisulfite solution to destroy residual chlorate in my sodium perchlorate solution before using KCl to drop out potassium perchlorate from the solution. Testing was required to confirm the chlorate was absent before adding the potassium chloride solution. I avoided the use of iron sulfate because I didn't want anything added that wasn't already there (it's like adding contaminants). The sulfates added are easily removed (from the electrolyte after the perchlorate is dropped out) with calcium chloride solution which drops out (low solubility) calcium sulfate, leaving sodium chloride solution if the reaction is balanced. If you plan to use potassium metabisulfite solution, KOH is a good choice of alkali to use for neutralizing the resulting acid. WSM Edited October 14, 2017 by WSM
WSM Posted October 10, 2017 Posted October 10, 2017 (edited) I know that you have to add the KCl slowly, but if you use a chlorate destruction method that generates dangerous gases, is everything fine if you just stay outside?what do you if you get that nasty gas? I did all the reacting in solution. When I added KCl solution to the purified (the chlorate was removed) NaClO4 solution, it was all at once and the KClO4 dropped out immediately as fine white powder and the beaker looked like it was full of milk till the crystals started to settle in the solution. I vacuum filtered the KP out using slow grade filter paper because of the fine particle size of the precipitated perchlorate. I suggest at that point to soak the wet KP mass in distilled water and re-filtering it as a better method of removing residual sodium contamination, than my method of rinsing the crystal mass in the vacuum filter with pure water. Using just a rinse didn't work as well as I had hoped, and I think a soak and subsequent vacuum filtering will work better to make your KP sodium-free. Good luck. WSM Edited October 11, 2017 by WSM
Recommended Posts