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Author: Subject: unconventional sodium
JJay
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[*] posted on 28-4-2017 at 00:22


Tomorrow, NurdRage is uploading his video on his new technique for making sodium. I can hardly wait.

C9-5eH0V0AALMqO.jpg - 292kB




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j_sum1
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[*] posted on 28-4-2017 at 02:24


Woohoo!
I think I will buy a few hundred grams of Mg in readiness!
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[*] posted on 29-4-2017 at 05:20


And, If I am not mistaken, I think this is the definitive work.
https://www.youtube.com/watch?v=jCrFFVVcPUI

Kudos to Nurdrage for his efforts. This really is the most promising thing I have seen in... well ever. It looks so much tidier than electrolysis of molten NaOH or any other methods I have seen.
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JJay
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[*] posted on 29-4-2017 at 11:47


Definitely very cool. I am going to have to make some dioxane when I get my fume hood built.



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[*] posted on 9-6-2017 at 12:56


Likewise, JJ. Although I'll work outside for it instead and wear hazmat gear in place of the hood, for this, considering that the initiation of the magnesiothermic reduction is not something one would want indoors. Happen to have plenty antifreeze that was going to be used for making perc, during a time when no chlorocarbons were available, but now plenty dichlor is to hand when needed, less can go on to be chlorinated w/ Zn/HCl, trying Nurdrage's dioxane method for Na separation (and will try with KOH also), got everything needed to make a go at it, just as long as the antifreeze is ethylene glycol rather than DEG as is sometimes to be found. Although I think I picked up some EG specifically, about a gallon of the stuff.

This is a great discovery, my compliments to Nurdrage for this. Looks like it beats the absolute piss out of the various rather touchy electrolytic processes.

How prone is 1,4-dioxane to peroxidation compared with diethyl ether, diisopropyl ether, and THF? for longer term storage of a quantity of dioxane that would be dedicated to this particular purpose, storage over sodium after argon sparging and degassing under vacuum, followed by an argon blanket over any headspace in the 1,4-dioxane ought to reduce and eliminate peroxides as formed should it not? so if stored over a few nuggets of Na, can the dioxane not be continually recycled, since refluxing over Na (and the dioxane batch being dedicated specifically to magnesiothermic Na or K production), it would get regular treatment for peroxides as essentially a side bonus of the process itself taking care of any formed peroxides should it not?

And two other questions-what is the shelf-life of 1,4-dioxane inhibited with a little BHT or BHA, with or without sodium? And uninhibited dioxane if not otherwise treated, how long does significant peroxidation take, roughly?

Have you considered, after first pre-drying the dioxane, using an argon blanket over the liquid 1,4-dioxane and storage under Ar to increase shelf life?

And when using Mg powder (mine is, IIRC 400 mesh, possibly 500) how manageable is the reaction in comparison with that using Mg swarf/turnings? does the fine grain size not result in a dramatically faster, more energetic reduction of the caustic? I'd sooner nnt have any rapid deflagration/flashover when attempting this.

I noticed, nurdrage, that he distilled the dioxane to dryness. This is something that I have always had drilled into me, as something never to do with ethers, does this apply to freshly treated (immediately before use) ethers, when treated for peroxides and distilled under a current of inert gas. Ordinarily distilling ethers to dryness is or can be dangerous because any peroxides formed already are concentrated and can pose a significant hazard if present, since once concentrated down there is much less solvent to peroxide ratio, increasing the potential for a big mess that one really wouldn't want occurring in one's glassware, and less still doing so whilst the experimenter is within range of flying razor sharp glass fragments.
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[*] posted on 9-6-2017 at 19:18


I honestly can say that the risk if peroxides is almost zero if the peroxides are stored over a small amount of sodium and kept in a tightly sealed bottle. I use Boston round bottles (from Dr.Bob, no less!) to store the relatively small amount of peroxide I have, but really any airtight bottle should work. As for the speed of the reduction, once I tried burning sodium hydroxide with magnalium (before the whole NurdRage sodium process came out) and using 200-325 mesh magnalium and coarse to medium hydroxide, and it burnt hot and even after cooling, reacted vigorously with water. Therefore, I think that with very fine magnesium and powdered sodium, you will boil off some of your yield.
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