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Triflic Acid
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[*] posted on 15-5-2021 at 08:42
Making Sodium, a new method?


Would it be possible to dissolve sodium chloride in a solvent such as 1,4 dioxane, and then electrolyze to get sodium metal? I need some sodium metal to follow a patent to make tetra-ethyl-ortho-silicate. Buying it is out of the question for me because of cost :(



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phlogiston
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[*] posted on 15-5-2021 at 09:03


This has been discussed in previous threads on sodium production. Not sure about 1,4-dioxane. IIRC propylene carbonate was considered a promising solvent for this purpose.

Regardless, figuring out a new method to produce sodium is going to be much more expensive than simply buying it, or following an established method. You could probably improvise some sort of Castner cell to make a small quantity somewhat cost-effectively.

So, if making the sodium is not a fun challenge to you and you just want some for a higher purpose, consider flipping burgers or delivering newspapers for a while and just buy some.

[Edited on 15-5-2021 by phlogiston]




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Keras
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[*] posted on 15-5-2021 at 09:09


Why don’t you use Nurdrage method?

I’m not certain 1,4 dioxane would be appropriate as a solvent. Does sodium chloride dissolve in it, in the first place?
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Swinfi2
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[*] posted on 15-5-2021 at 09:12


I tried a Craster cell outside, decent ppe, googles, labcoat and a loose brick wall and still got a small 2-3mm scar from the constant explosion and molten NaOH. And I didn't recover any usable amount. I would have enclosed it but was more worried about larger explosion potential... I would recommend a face shield at minimum but honestly I'm not trying this method again.

If you have dioxane and menthol look at nerdrage's work on sodium.
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Triflic Acid
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[*] posted on 15-5-2021 at 09:20


Making sodium seems fun as well, and the next few things that I want to do all require sodium. So, making it would be nice. 1,4 dioxane does dissolve salt, so I think that I will try that. I also am paranoid about a fire starting, so Swinfi's post scared the crap out of me. I live an a place really prone to forest fires, and don't want my face in the local newspaper :P I also don't feel safe leaving something at 200C overnight, which rules out nurdrage's method too. So, I think I will try this sometime next week, once I make some dioxane. Proplyene carbonate seems too hard to make for me. Ethylene carbonate seems easier, but the workup seems equally challenging.



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[*] posted on 15-5-2021 at 11:15


Same I've had molten lye explode on me i got lucky it didn't hit me. When I did the experiment I got a little bit of sodium. We threw the little pea sized sodium it in water and watched it zip around my buddy told his teacher and he was surprised he had made sodium metal this was in high school 12 years ago so times were different.
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[*] posted on 15-5-2021 at 21:40


The sodium hydroxide - magnesium thermite type reaction followed by 1,4 dioxane workup seems the way to go if you don't want to deal with the longer menthol procedure.

Nurdrage has videos on this.

If you really want to try the electrolytic method, potassium chloride is much more soluble in 1,4 dioxane.
Also when I say much more soluble, by most standards salts are insoluble in 1,4 dioxane (0.000425 mol/L).
I would also be concerned about chlorination of the 1,4 dioxane if you could get it to work.
It is already a probable carcinogen, adding chlorine to the mix sounds like it would be more toxic.
But if you have good ventilation and a way to dispose of chlorinated hydrocarbons safely, then it is worth a try.

The following link has solubility data for sodium and potassium chloride in 1,4 dioxane and water systems.
At 100% dioxane, it really isn't soluble.
https://link.springer.com/article/10.1007%2Fs10953-006-9061-...

sodium hydroxide might be more soluble in dioxane. I could not find a good reference but it is almost midnight.
This would eliminate the chlorination issue.
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Deathunter88
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[*] posted on 15-5-2021 at 23:15


Unless you have the magnesium powder and dioxane, just buy it, it will be cheaper and less work. It's not that expensive. https://onyxmet.com/index.php?route=product/product&path...
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[*] posted on 16-5-2021 at 07:15


Solubility isn't the issue, you may get solubility but the solution likely will not conduct or will have vanishingly low conductivity. Depends on if the material actually forms ions and if they coordinate. The classic example for sodium is the electrolysis of sodium chloride / aluminum chloride complex in nitrobenzene. Apparently you need to fuse the sodium chloride / aluminum chloride and this makes Na+ / AlCl4- ions in the nitrobenzene which will conduct charge whereas NaCl dissolved will not. Again though, the conductivity if it is there is usually much lower in organic solvents than aqueous solutions, sometimes you're lucky to get 0.0002A going through a solution which of course leads to very... very ... long reaction times.

Re: Castner Tigel cells - the difficulty with these is the narrow range of temperature for proper electrolysis. Too hot and your sodium reacts / dissolves in the melt and you get nothing. Too cold and you freeze the whole thing. The only success I've had with molten NaOH electrolysis is the small (multi-gram) scale. When I tried to take it up to 5 kg (or even 500 g) of melt I wasn't able to get the control I needed and just started fires and wasted starters.




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[*] posted on 16-5-2021 at 07:33


For the production of alkali metals by electrolysis I have always thought that the bis(oxalato)borates, easily prepared by heating the metaborates with oxalic acid, should of course be the salts of choice; the ion is exceptionally non-coordinating and gives high solubility in organic solvents. Propylene carbonate and nitrobenzene are the only solvents I have heard support the high overpotential required, but if NaBOB dissolves in an ethereal solvent, it should probably be fine, I would imagine. (And what a fun name!)

However, I agree with everyone else saying that if you just want Na, use the established magnesiothermic method.




[Edited on 04-20-1969 by clearly_not_atara]
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Triflic Acid
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[*] posted on 16-5-2021 at 08:08


In the end, for the use I need sodium for, I just need an alkali metal. So, I'll probably try to use lithium from batteries for the time being. I'll also try out the electrolysis when I have time.



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JuliusCaesium
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[*] posted on 27-7-2021 at 11:34


Quote: Originally posted by Triflic Acid  
Would it be possible to dissolve sodium chloride in a solvent such as 1,4 dioxane, and then electrolyze to get sodium metal?


I'm not sure if you've seen this video but a few years ago NurdRage on Youtube was able to make sodium metal using dioxane without electrolysis. Not sure if this is still applicable bc its been a few months but thought id share anyway. (link below)

https://www.youtube.com/watch?v=jCrFFVVcPUI
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[*] posted on 27-7-2021 at 13:01


I think there's an old thread on her somewhere about electrolysis for making alkalai metals in pyridine, but I haven't found it.

This was a thread by tashaggua, or something like that.

I'm not sure of the spelling, but he used to include a lot of long discursive personal stuff about being Kanner's autistic in his posts and said he was an avid amateur mycologist with a gammy leg.

I mention these traits in hope that they will remind somebody who's been here a while as to who I'm talking about.

Edit: But yeah, scavenging some lithium from a battery would probably be the smart move.


[Edited on 27-7-2021 by SWIM]




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[*] posted on 27-7-2021 at 13:50


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[*] posted on 28-7-2021 at 04:53


excellent point ark



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[*] posted on 24-10-2021 at 12:09


I messed up my nickel crucible so I though it might be a good idea to resurrect it in a castner cell, it was a fun project! nothing was particularly difficult, there was a description on this forum somewhere, I followed only the steps in the design that made sense, most of the things are not so critical I think, and indeed there are small bangs at the first 1hour if you are impatient, but these are not so violent to splash molten NaOH around. Attached pic on the anode and collector tube, and Na after ~6hours run.

IMG_3839[1].JPG - 456kB IMG_3879[1].JPG - 1.7MB
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