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Alastair
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Sodium is paramagnetic, so "is only attracted when in the presence of an externally applied magnetic field" (wiki)
Maybe it would just stick to the magnet leaving behind most of impurities. But that is just a guess. It might not work with simple magnets, and i for
one wont test it right now, though i wish i could.
Just it seems to be an idea worth trying, if one doesn't want to distill.
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watson.fawkes
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Quote: Originally posted by Alastair  | | Sodium is paramagnetic, so "is only attracted when in the presence of an externally applied magnetic field" (wiki) |
The strength of that interaction is minuscule. It also decreases with temperature. Plus you're talking about a liquid, not solid, so
there's yet another source of spin disordering and an even lower strength of interaction.
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Alastair
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| Quote: Originally posted by watson.fawkes | | The strength of that interaction is minuscule. It also decreases with temperature. Plus you're talking about a liquid, not solid, so there's yet
another source of spin disordering and an even lower strength of interaction. |
I won't start a pointless discussion about sodium being a solid.
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watson.fawkes
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That's good, because in all the elemental
sodium syntheses I've seen here, the sodium comes out at elevated temperatures, as a liquid.
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Alastair
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| Quote: Originally posted by watson.fawkes | | That's good, because in all the elemental sodium syntheses I've seen here, the sodium comes out at elevated temperatures, as a liquid.
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That's good, now you can start a chemistry/physics revolution and change all the literature on sodium, and everything else that liquifies just below
100C. Good luck 
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watson.fawkes
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| Quote: Originally posted by Alastair | | That's good, now you can start a chemistry/physics revolution and change all the literature on sodium, and everything else that liquifies just below
100C. |
Are you actually asserting anything? I can't tell. Otherwise I'll have to assume you're trolling.
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Alastair
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You can assume whatever you want. I feel that this "dialogue" is getting quite boring for others to read. If you think it is a big problem to cool
sodium down to room temperature, you can aswell go on theorizing about it. My point was just to propose an idea for someone who would actually try it,
wouldnt hurt i think? Anyway, thanks for your oppinion.
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watson.fawkes
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| Quote: Originally posted by Alastair | | If you think it is a big problem to cool sodium down to room temperature, you can aswell go on theorizing about it. My point was just to propose an
idea for someone who would actually try it, wouldnt hurt i think? |
I see. Cool it down and lock in all the
inclusions into a solid matrix where you're going to get zero separation. Well, that won't work either.
So "someone who would actually try it", SWWATI, is apparently not you. Well, now I know. At least now I realize I'm not trying to help you, but rather
the anonymous future reader who might not realize that they'd be wasting their time.
SWWATI, while not as obnoxious as SWIM, has at least a certain responsibility to make sure your proposal isn't totally hare-brained. If you're going
to do armchair chemical engineering, then, at least have the grace to put a sanity check on your idea, like, oh, calculating some numbers.
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metalresearcher
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Last week I got sodium by heating Na2CO3 + C in a steel tube to 1200C but capturing under oil did not work yet.
<iframe sandbox width="640" height="360" src="http://www.youtube.com/embed/9l_DojAugyg" frameborder="0" allowfullscreen></iframe>
And the same for K2CO3 + C:
<iframe sandbox width="640" height="360" src="http://www.youtube.com/embed/nUQNjO32vyQ" frameborder="0" allowfullscreen></iframe>
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m1tanker78
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Nice demo MR! I've had some success in the past from condensing sodium vapor on a cooled metal surface. The vapor was generated in an overheated Downs
cell (the reduced sodium boiled off instantly) and collected inside of a tube. Collecting the sodium in oil is definitely worth a try but you may find
quite a bit gets trapped in the retort outlet.
How are you drying the carbonate salts before charging the retort?
Tank
Chemical CURIOSITY KILLED THE CATalyst.
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aliced25
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Right, I posted in the wrong forum as I was a little stunned by this video (http://www.youtube.com/watch?v=seSg_GWj1b0).
Now, there are some serious problems with what he is doing, but the basic procedure is exciting. If Mg can reduce NaOH, then if we heat the material
in a furnace/kiln - a propane furnace will hit the right temperatures, then a finely divided, briqueted form of NaOH (fused) and Mg could be heated
under a mild vacuum and distilled (the boiling point of Na is 883C at 1Atm, so it would be considerably less under vacuum, at 20mtorr it comes over
between 300-350C, (http://www.osti.gov/bridge/servlets/purl/4478378/4478378.pdf) we won't be going that far, but 500-600C is likely with a normal single stage
sliding vane pump at 10pa (or 75mtorr).
It is a variant of the Pidgeon Process, which works with Magnesium (Silicothermic), Calcium (aluminothermic), Lithium (Aluminothermic/Silicothermic or
Magnesiothermic) and presumably quite a lot of other chemicals.
Attached is a paper on the Design of a Distillation apparatus for Lithium, the v-shaped apparatus looks like something we'd use - although, if we had
a furnace with a gas take-off tube for the gaseous metals, then that could be cooled enough to allow the liquid metal to run down into the condensing
area.
Attachment: Rogers.Viens.Effect.of.Pressure.on.the.Refining.of.Lithium.by.Distillation.pdf (465kB)
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Attachment: Kroll.Schlecten.Laboratory.Preparation.of.Lithium.Metal.by.Vacuum.Metallurgy.pdf (373kB)
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Attachment: Morris.Pidgeon.The.Vapor.Pressure.of.Lithium.in.the.Reduction.of.Lithium.Oxide.by.Silicon.pdf (202kB)
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Attachment: Epstein.Howland.The.Distillation.of.Lithium.Metal.pdf (506kB)
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aliced25
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This shit, Self-propagating synthesis, is insane. Microwaves with a susceptor (generally SiC powder packed between two crucibles) have been used to ignite
what are essentially thermite mixtures, which burn in a vacuum/gasless environment, producing everything from TiC and other refractories to NiAl Alloy
(useful). I suspect they could be harnessed for the preparation of alkali metals, as the volatile components of various Pidgeon-type processes - just
put a hole in the top of an old MW, insert a large crucible, then pack it with SiC, then another crucible, with a cover that can hold a vacuum (no MW
are reaching this, so bolt-down lids would be a good idea).
This is some sick shit, thermite in a MW - perhaps we can make Si without needing Sulfur (YAY). 
From a Knight of the Realm: "Animated movies are not just for kids, they're also for adults who do a lot of drugs." Sir Paul McCartney
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blogfast25
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Sure. That thermite is slightly exothermic, so if you heat it enough you'll end up with molten alumina and molten Si.
The Standard Enthalpy of Reaction for SiO2 + 4/3 Al === > Si + 2/3 Al2O3 is about - 212 kJ/mol, that's quite a bit for free. Provide the missing
heat (to get to about 2,500 C) with MW and Bob should be your uncle. Just don't expect chip grade!
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aliced25
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Don't want chip grade, what I want is a reductant for various other metals, including lithium, possibly strontium, and especially calcium. I'd also
like to make the aluminium silicon alloy the Russian's used to reduce KCl with (http://www.dtic.mil/dtic/tr/fulltext/u2/a359639.pdf). What is your idea, first go with a propane kiln and something like this (http://www.scribd.com/doc/123531537/Magnesium-silicothermic-...)? A simple rotary-vane pump should get enough vacuum, if not we need additional
heat. Working with thermite mixtures we run into the issue that even under vacuum they start a self-sustaining combustion reaction (http://en.wikipedia.org/wiki/Self-propagating_high-temperatu...) which will rapidly reach and breach the ability of most metals to contain the
reaction with some products.
But done properly, this is possibly the best route for the home scientist to get access to some serious quantities of a variety of metals, no
electrolysis, no exact heating - if the SHS kicks in heating isn't the issue anymore anyhow- just high quality distilled metals.
[Edited on 4-6-2013 by aliced25]
Attachment: Heat.Resistant.Concrete.for.Vacuum.Distillation.Furnaces.pdf (519kB)
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[Edited on 4-6-2013 by aliced25]
Attachment: Selmanoff.The.Design.and.Some.Construction.Details.of.Two.Laboratory.Vacuum.Furnaces.for.Casting.Metals.pdf (427kB)
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watson.fawkes
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| Quote: Originally posted by aliced25 | | Don't want chip grade, what I want is a reductant for various other metals, including lithium, possibly strontium, and especially calcium.
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If all you want is a source of silicon for reduction, there's no need to use elemental silicon. If crude
silicon works for you, then ferrosilicon should as well.
There are four low-melting eutectic points, that is local minima on the phase diagram. The one with the greatest percentage of silicon is the eutectic
of FeSi and Si, at around 60% Si. But the whole range from ~ 50% Si to 60% Si has a melting point at 1207 - 1220 °C, a couple hundred degrees
lower than that of Si itself at 1414 °C. This is rather easier to get to, as the T4 ratio is 1.8 (that's ratio of radiative heat
loss).
And it's a lot easier to make an arc furnace than screwing around with microwaves. Welding rods, castable refractory, and an ammeter (to know when to
push the rods in) is all you really need. At the materials are dirt cheap: sand, carbon, and steel scrap.
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blogfast25
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| Quote: Originally posted by watson.fawkes | If all you want is a source of silicon for reduction, there's no need to use elemental silicon. If crude silicon works for you, then ferrosilicon should as well.
There are four low-melting eutectic points, that is local minima on the phase diagram. The one with the greatest percentage of silicon is the eutectic
of FeSi and Si, at around 60% Si. But the whole range from ~ 50% Si to 60% Si has a melting point at 1207 - 1220 °C, a couple hundred degrees
lower than that of Si itself at 1414 °C. This is rather easier to get to, as the T4 ratio is 1.8 (that's ratio of radiative heat
loss).
And it's a lot easier to make an arc furnace than screwing around with microwaves. Welding rods, castable refractory, and an ammeter (to know when to
push the rods in) is all you really need. At the materials are dirt cheap: sand, carbon, and steel scrap. |
Ferrosilicon was mentioned in the other thread.
Ferrosilicon can be made easily by mixed thermite (Fe2O3 + SiO2 in the desired ratio, + Al and CaF2). The Fe2O3 acts as the heat booster to provide
the 'missing heat' for the straight SiO2 thermite. I've done this with good results a few years ago. Because various FeSi mixtures are more dense than
pure Si, you also get much better gravitational separation which tends to be a problem with sulphur assisted SiO2 thermites. Not to mention the H2S!
FeSi globules from aluminothermy: still quite uncorroded after so many years:
If it was me, definitely propane kiln.
Self-sustaining reactions obviously wouldn’t work here in most cases. It’s PRECISELY not self-sustaining reactions that should be the target of
this ‘reactive distilling’.
[Edited on 4-6-2013 by blogfast25]
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aliced25
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Precisely, these reactions aren't self-sustaining, they need vacuum in order to proceed. @Watson.Fawkes, we are trying to avoid the need for an arc,
for one thing it is going to seriously complicate building a vacuum container and for other, external heat is applied to cause the reaction to kick
in.
For mine, if we can make pure silicon, we can make pure silicon, it is about the same price on pyro sites as Ferrosilicon anyway, the only thing that
has put people off it in the past is the slag forming H2S. If external heating can be used to kick the fucker off, then a simple Al/SiO2 reaction with
Si and Al2O3 as the slag would be fucking brilliant. The less crud in the pot the better when trying something new out is how I look at it (although
Pidgeon, et al, did use Ferrosilicon for the reduction of both Lithium and Magnesium, because it was cheaper than Al - not our problem, for us Al is
significantly cheaper, as is Mg for that matter).
An externally heat-ignited thermite mixture, would presumably have very similar effects on crucibles as the normal thermite reactions, so I would
suggest that any vacuum vessel be designed to have a single-use crucible, that is cheap and expendable and can be placed in there easily (ie. the
thing should be able to be pulled apart, in fact modular would be great). The difficulty is, how to we get the external heat through an expendable
crucible to the reagents, sufficient to raise them to initiation temperatures? How do we get a metal that will allow us to push that much heat through
it without melting/deforming under vacuum? I know the Russian's used a Tungsten wire to initiate the SHS mixtures, which could be conceivably pushed
through the vacuum housing and potentially through a small hole in the base of the expendable crucible. But that gets away from the propane idea into
electrodes.
A lot of questions to be answered yet, not to worry, we have the collected literature of NASA, the US Military and the USSR's best Scientists to help
us answer it. A straight crucible, made of something like alumina (or porcelain
- such as a porcelain vase/cup) that costs fuck all, would be the first part. SS to contain it, which would need to be vacuum sealed to the main
chamber (containing air/water cooled condenser and collection cup). I'm thinking flanges here, bolted flanges joining the two components with a
gasket.
I'm thinking if we keep the original small, then catastrophic failure of any component would be no more dangerous than a normal thermite reaction. A
vertical design for the area going into the furnace, simplifying the system and probably an angled condenser coming out of the area above it to both
the collection cup and vacuum take-off (like a normal pot-still). I think given the range of materials this will be tested with, from alkali metals to
phosphorus, SS is going to be the best option, I'm just worried about it's ability to cop the heat at the furnace end.
[Edited on 5-6-2013 by aliced25]
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watson.fawkes
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| Quote: Originally posted by aliced25 | | we are trying to avoid the need for an arc, for one thing it is going to seriously complicate building a vacuum container and for other, external heat
is applied to cause the reaction to kick in. |
I didn't say at all that you'd use the same reactor. Use an arc
reactor for lots of ferrosilicon, which you take out and use somewhere else.
Edit: typo. clarity.
[Edited on 2013-6-5 by watson.fawkes]
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aliced25
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Oh ok, my mistake
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watson.fawkes
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May 1933 article from Modern Mechanics
Experimental Arc Furnace Melts Anything
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aliced25
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Yep, and there is this one (cited in the Phosphorus reduction papers). The difficulty I foresee is the circuit (I'll need help on that) and how to
modify it for vertical operation (otherwise we'd be restricted to what could be put in a boat inside the furnace).
BTW Could you grab that entire paper?
PS Here is another laboratory furnace by Kroll, et al, (pdf) for the production of Zirconium.
Attachment: Bryan.Mehring.Ross.An.Electric.Graphite.Resistance.Furnace.pdf (277kB)
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[Edited on 6-6-2013 by aliced25]
Attachment: Evans.A.Vertical.Vacuum.SplitTube.Graphite.Resistance.Furnace.pdf (251kB)
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Attachment: Kroll.etal.Recent.Progress.in.the.Metallurgy.of.Malleable.Zirconium.pdf (912kB)
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aliced25
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Stauffer has probably got the simplest furnace design I have ever seen for this (on page 3/11) - a simple burner, in a kiln/furnace with bricks, and a
condenser attached to a vacuum pump.
He uses Spodumene with ferrosilicon and uses calcination, which is going to be a headfuck and a half, given Li makes up only 3% of Spodumene even
minor screwups will lose half your yield.
At the same temperatures though, using Lithium carbonate ==> Lithium Oxide (by thermal decarboxylation - mix with with Calcium Carbonate and they
both decarboxyalate at a lower temperature I read somewhere), then silicon/ferrosilicon or aluminium to get lithium. Looks awfully simple, a decent
vacuum would be needed, as would a propane torch/meker burner.
Like I say, start from the more expensive lithium carbonate which has a way higher percentage of lithium and save the fucking around (http://digitool.library.mcgill.ca/webclient/StreamGate?folde...). Same setup apart from that. As CaO is going to be needed, and there is
apparently a eutectic (according to one paper), it might need to be looked into further. In the presence of Al powder, it undergoes decomposition to
the oxide without being wetted (too low a temperature) at 700C or so.
Attachment: Stauffer.Vacuum.Processes.for.the.Production.of.Lithium.from.Spodumene.pdf (393kB)
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Attachment: Ktakkherman.Emelkin.Pozdnyakov.Production.of.Lithium.Oxide.by.Decomposition.of.Lithium.Carbonate.in.the.Flow.of.a.Heat.C (188kB)
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Attachment: Vlasov.Poroskova.Sinetering.of.Calcium.Carbonate.in.the.Presence.of.Lithium.Carbonate.Additive.pdf (240kB)
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Attachment: Bazhenov.etal.Study.of.the.Process.of.Dissaciation.of.Lithium.Carbonate.in.the.Presence.of.Aluminum.Powder.pdf (273kB)
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aliced25
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Probably the best way to work this is to try out the preparation of Calcium metal from a much cheaper ore, similar reaction, similar product, just a
cheaper ore.
Attachment: Di.Wang.Tao.Feng.A.Novel.Vacuum.Aluminothermic.Reduction.Lithium.Process.pdf (305kB)
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Attachment: Lebedev.Shishkina.Dmitriev.Preparation.of.48Ca.and.its.Use.in.Experiments.on.Synthesis.of.New.Superheavy.Elements.pdf (150kB)
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Attachment: Loomis.The.Production.of.Metallic.Calcium.by.Thermal.Reduction.pdf (1.3MB)
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aliced25
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These seem to take me over my file size, so I'll attach just two then the other one
[file]23831[/file]
[file]23827[/file]
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halogen
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http://link.springer.com/article/10.1007%2FBF00608791
I don't believe it! So what do you get on the other side, products from oxidation of propylene carbonate? Perchlorate?
[Edited on 8-8-2013 by halogen]
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