Lab Notes - Perchlorate Process Optimization

[@chemistryofquestionablequa6252]

You can extract the NaClO4 with acetone as well. When I’ve done this I’ve used only enough heat to have a slow rate of bubbling and it all seems to convert very near the end of heating rather than over the span of the reaction, not sure why.

[@MIH0319]

Lol in China acetone is restricted for some reason so I can't get it

[@chemistryofquestionablequa6252]

@@MIH0319 I forgot you were in China, that’s such a weird restriction.

[@philouzlouis2042]

@@MIH0319 Probably due to the unfamous peroxide used by Ter-Ro-Ri-St CycloTriAcetonPeroxide (CTAP) wrongly named C A T P

[@达闻西-o5e]

Nice job. How about your Ostwald going? I like that very much.

[@MIH0319]

I already bought a bunch of nitrates so I don't think I will rely on my Ostwald on making nitric acid. However I probably will try the process again just for fun

[@7hunderstorm242]

Very nice ! What are you going to use the NaClO4 for ?

[@MIH0319]

For ammonium perchlorate and pyrotechnics, if everything goes right.

[@goiterlanternbase]

Who needs to buy a heating mantle🏆

[@thorium_labs]

Cool video + can this process be used to make KClO4?

[@chemistryofquestionablequa6252]

Yeah, if you use a mixture of NaClO3 and KClO3 you actually get better yields.

[@MIH0319]

@@chemistryofquestionablequa6252 Well not exactly. KClO4 has poor solubilities in organic solvents so you probably can't extract it out very easily and lose a bunch of yield.

[@chemistryofquestionablequa6252]

@@MIH0319 you can’t do the extraction the same way, for KClO4 you use water, but the disproportionation part is exactly the same.

[@MIH0319]

@@chemistryofquestionablequa6252 Right, but will a water extraction separate the KClO4 from the remaining KClO3 cleanly or multiple extractions (or crystallizations) are required?

[@NinjaChemistChannel]

With kclo4 you dot need to use organic solvents because of poor solubility. Single recristallization from boiling water works best, most of kclo4 will precipitate on cooling.

[@EdwardTriesToScience]

another optimization is eutectic formation by using 1:2 ratio of KClO3:NaClO3 which lowers the reaction temperature (allowing for disproportionation but not decomposition) and even when overheated yields 80% or so source kzbin.info/www/bejne/rIGmoJKgeaaCqJY (this guy specializes in electrochemistry and chlorate/perchlorate if you havent seen him before)

[@MIH0319]

I've came across this video in my research and it seems promising. I'll try the method in my next perchlorate vid

[@Exotic_Chem_Lab]

you should never use more than 5.5V for chlorate cell. also measure the surface area of MMO (both side)and multiply it by 0.2 to get the current that u need to feed the cell

[@MIH0319]

The voltage displayed on the module was the output of the power supply and isn't the actual voltage across the cell. I've connected a resistance wire in series with the cell to control its voltage and current

[@Exotic_Chem_Lab]

@@MIH0319 you should make a small PbO2 electrode.... Its much better for making perchlorate. Its relatively easy to make... You just need NaOH and PbO and current control.

[@gabrielsanchezdominguez3256]

​@@Exotic_Chem_Lab It is very easy, but it requires a lot of time and control over the pH.