Thinking I might do a synthesis of some 1,4-dioxane (a cyclic diether solvent, having two, two-carbon chains linked to each other at each end by a pair of oxygen bridges oriented parallel to each other), all I'll need for it is antifreeze (ethylene glycol) an to drip it into boiling concentrated sulfuric acid, distilling off the dioxane as it forms. Got about 5 liters of the stuff, undiluted (which is better since then I won't have to distill the water out of it before it forms, since the sulfuric acid cyclization reaction works by dehydration, water content would be detrimental and consume some of the sulfuric. A lot of antifreeze is sold as a ready-made mixture containing about 60-70% ethylene glycol, but I found a place that has it, for this purpose, more or less considerable as pure, its treated with traces of bitrex to warn people off consuming it and poisoning themselves, put kids off etc. and dyed pink, but that won't follow through the distillation, and there is some chance any dye might be destroyed by contact with boiling hot 96-98% sulfuric acid anyway. So the dioxane will come over cleanly. Need some for two reasons-mainly, I want some sodium, and due to storage and shelf-life considerations I'd sooner keep the brick I have in one piece, in its double-layer of hermetically sealed packages in its vac-packed, oil-filled inner liner, inside the sealed bag full of inert gas thats kept in. Under dried mineral oil it still, very slowly, does degrade. It is slow but I'd rather not have it happen just sitting on the shelf, since I only need maybe 15g out of the 100g brick of the stuff I have. So the plan is to do a thermite-like reaction using magnesium powder to reduce caustic soda, stick the resulting slag in a kitchen blender purged with argon (not vital but it should improve the yield) and powder it, then boil it up under dioxane, which just happens to have the right surface tension and other ideal characteristics, such as for example, being unreactive with sodium, and negate the need for shielding with inert gas due to its combination of fairly high boiling point, and when boiling, it generates a dense cloud of dioxane vapor which effectively pushes out and excludes air from entering and igniting the sodium. I'll probably end up with more than I need, which since it can effectively be made on tap, without resorting to the fiddly, current- and voltage-sensitive, temperature sensitive messy high temperature electrolysis of molten caustic soda or molten salt, in a divided cell to prevent the chlorine from backwashing towards the formed sodium and making a big fucking mess This way, its melted out of the magnesium oxide slag, which is impregnated with quite a decent level of sodium metal, after blending it to a powder, all under the unreactive solvent, which can be recycled and recycled and recycled by distillation, storing it over a small piece of sodium to prevent it peroxidizing in storage (ethers have a nasty tendency to formation of organic ether peroxides and hydroperoxides. The hydroperoxides apparently are somewhat sluggish, deflagrating but they are intermediates in formation of the extremely sensitive alkylidene peroxides, of which it takes just a few mg to shatter a flask into a storm of razor-sharp fragments, and needless to say, you don't really want to be around if it does. So there are methods around developed as countermeasures, for stabilizing ether-type solvents (which 1,4-dioxane is) and for destroying any peroxides in-situ by storing it over various materials which destroy the peroxides as and when they are formed so they never get the chance to build up, as well as for testing the ethers for peroxide content and if discovered to be lurking, to destroy them. Storage over Na metal chips and a bit of copper powder or twists of copper wire should both keep the dioxane dry and destroy any peroxides as they form. Convenient of course being able to use sodium for the drying and peroxide-destruction in storage to prevent them building up, since Na is what I'd be using it for making (as well as potassium and the other alkali metals of course)
Not that straight after making it there would be a peroxide problem anyway, it happens via the intermediate hydroperoxides, and both form via reaction with the oxygen in air, slowly, so its a long term storage problem rather than an immediate hazard, unless the ether is already old, has already been stored, and the owner has neglected to regularly perform testing to check it for peroxidationn and destroy any peroxides found if present. Since I like my lab in one piece, and want to keep my hazardous chemicals fridge in the same state, of course, I make sure to test and rid any ethers I use of peroxides on a regular basis.
The dioxane separation method though looks neat as hell for alkali metal production. I've never done it, not yet, anyway, but I've seen somebody's videos of it done, from the thermite type reaction with powdered lye and magnesium, to the production of the 1,4-dioxane and the separation of the pristine sodium metal from the MgO slag. Looks great. Turns it from chunks of grey, dirty, cement-like rubble to big round blobs of shiny clean sodium metal using just a hotplate for heating (Na has a pretty low melting point, which makes it feasible to do the job under dioxane, which for an ether is reasonably high boiling, at 1 degree 'C higher than the BP of water)
Methinks I'll have my work cut out for me for a while, although in a good way since it'll be fun.
