Greetings fellow nerds.
Doing another lab notes video on my project on making sodium metal.
As you already know by now i've been making sodium metal by the alcohol catalyzed magnesium reduction process and have been very successful so far.
I've been able to refine the techniques for recovering sodium and i've also been able to solve the troublesome glassware destruction problem.
Basically i had to dry the sodium hydroxide with sodium metal.
Overall things look pretty good.
Now it's just an optional matter of exploring the chemistry a bit more and maybe find a few more ways to streamline and optimize the process.
In this video i wanted to focus on finding an alternate way to dry the sodium hydroxide or jumpstart the reaction.
Using sodium metal is the best way since sodium just adds to our yield and doesn't contaminate our process or create additional waste.
After we get an initial jumpstart quantity of sodium and use it make more sodium we can just continually feed forward into subsequent runs.
But we still had the problem of getting the initial charge of sodium.
It wasn't too much of an issue though.
As we can just make it directly using the thermochemical dioxane process.
But for those amateurs who don't want to bother their neighbors with giants clouds of caustic smoke a pure wet chemical process would be desirable.
Even if it's more expensive and cumbersome, all we need is an initial jumpstart.
So my first idea was a rather crazy one and that was to dissolve a small portion of magnesium in methanol and make magnesium methoxide
and then use that to react with a small portion of sodium hydroxide in methanol.
Overall what would happen is that we'd make a mixture of magnesium oxides and sodium methoxides
and this in turn could be used to consume the water in a larger portion of sodium hydroxide.
Yeah i agree it was a rather stupid and crazy idea
but i'm of the philosophy that 5% to 10% of your research ideas should be crazy because that keeps you from being trapped in a rigid framework.
And once every year or so when your crazy idea does work it's awesome.
Unfortunately this wasn't one of them.
The magnesium methoxide and the sodium hydroxide solution formed a sol-gel that was really hard to dry out.
Oh well. Back to more mainstream ideas.
My next thought was to try and make sodium in a beaker.
Rather than avoid destroying glassware i thought we should attempt to make the cheapest sacrifice possible.
Beakers are very cheap compared to flasks with ground glass joints
so even if the beaker was destroyed that would be a much more acceptable sacrifice to get an initial charge of sodium.
So i ran the sodium production reaction using the alcohol catalyzed magnesium reduction approach in a beaker with a round bottom flask of water as a condenser.
It failed miserably and produced no sodium or reactive compounds.
I think the problem was air.
In all my reactions i always hooked up a bubbler to monitor progress.
This also prevents backflow of air into the flask.
But in a beaker I didn't have this so air could get in.
I think this reacted with any sodium produced and maybe also oxidized the alcohols.
So that was a failure.
To be certain i ran it a couple more times and also tried doing it with aluminum foil lining to reduce damage to the beaker in a separate line of inquiry.
It all failed, producing this thick goo of aluminum and magnesium oxides.
So for now i'm going abandon beakers.
But this doesn't mean it can't work.
Maybe making sodium a mason jar would be viable since they're designed to let gas out but not back in.
However, i'm not going to try this yet because i don't trust a soda lime glass mason jar to handle the extreme thermal stresses the reaction produces
as well as genuine borosilicate glass labware.
So let's move onto our new round of testing.
This is the flask for my next test.
I'm taking pictures now of before and after my experiments to document extremely subtle damage.
And this is going to be my new test apparatus.
I'm using a claisen adapter so i can connect a bubbler as well as insert a thermometer directly into the reaction mixture.
You might be wondering why i don't have a reflux condenser anymore.
I find that now that we're using much lower temperatures of around 200 celsius the baby oil evaporates very little.
Just the cooling action of the neck of the flask and the claisen adapter is enough to recondense it.
So we don't need the condenser anymore as long as we keep using the lower temperatures.
A small bonus of our chemistry that makes it even easier for the amateur to execute.
So for my next experiment i'm going to try using aluminum metal powder as the drying agent.
I had the idea for using aluminum metal after i realized in my last video
that the glassware destruction reaction generated water that i believe helped to cause further destruction and product loss.
The reaction of aluminum with sodium hydroxide is a water consuming reaction.
Although it does deplete some sodium hydroxide so we'll probably have less yield.
Anyway, after mixing in aluminum metal, sodium hydroxide, mineral oil and tertiary alcohol I inserted a digital thermometer and began heating.
I'm using an internal thermometer now to better track the internal temperature of the reaction mixture and make my results more reproducible.
Now that we've been able to lower our operating temperature down to 200 celsius small changes in temperature now have greater effects.
Anyway, i slowly ramped up the temperature from room temperature up to 200 celsius over the course of about four hours.
As you can see by the bubbling the reaction of aluminum and sodium hydroxide with water seems to be working and generating hydrogen.
Once i hit 200 celsius i held the temperature for another 4 hours and then let it cool to examine the flask.
And here we are at room temperature... This is not good.
This white clouding of the glass definitely wasn't there when we started and indicates the glass is being damaged.
This particular experiment is a failure.
Not to let an experiment go to waste i added magnesium anyway and still proceeded to try and make sodium.
This was to figure out if aluminum has a negative effect on the sodium production reaction.
I'm not sure if this is ultimately important
but i figured it was good data to have in case we decide to use aluminum vessels or other aluminum reactants in the future.
And after reacting for several hours we indeed did get sodium production.
It was slower than usual but that's probably because of insufficient water removal by the aluminum.
I processed the reaction as usual and i noticed that the aluminum doesn't mix in with the sodium.
This is a good thing actually and means that the sodium is relatively aluminum free.
And here is the cleaned flask.
The damage is there compared to the previous picture but actually quite small.
Maybe we can do better.
I think maybe i simply ran the drying step too fast.
Unlike sodium, aluminum does not liquefy at these temperatures so it would take much longer to react with the water.
So i setup another run using the same flask but this time ramped the temperature to 200 celsius over the course of 8 hours.
This time i didn't put in magnesium since we already know we can make sodium even with aluminum present.
So to save time i'm just going to focus on the aluminum drying.
And here it is after 8 hours and allowing it to cool down.
Looks good. Maybe it worked this time.
On a different note it doesn't seem like we're making sodium with just aluminum.
In theory it should be possible to make sodium from aluminum but it doesn't seem we have the right catalyst or temperature to make it happen. Oh well.
Now here is the flask after cleaning.
Okay looks like i blundered by using the same damaged flask as before as i can't tell the difference.
If there is damage it's very subtle.
But I suppose that's still an improvement over earlier.
So let me get a much better flask and try this all over again.
We mix aluminum powder, sodium hydroxide, oil and alcohol and ramp to 200 celsius over eight hours.
Flask looks pretty good.
And here it is after cleaning.
We're doing better but it's not perfect.
It's very hard to see on camera but there is degradation over here.
Nonetheless, while aluminum is not as good as sodium, it's still a very good drying agent compared to magnesium alone.
This level of damage is acceptable in my opinion as the flask is still fully functional.
But can we do even better than this?
Let me get another flask now.
First i'll fill with oil.
At this point i'm going to move on and try a new drying agent, lithium metal.
Lithium metal is actually not that hard to get.
It can be obtained from energizer lithium batteries.
While this is extremely expensive, and thus why i never considered it for making sodium earlier.
It only needs to be used once to dry the sodium hydroxide and jumpstart the reaction.
So making sodium from lithium is back on the table.
Now i already have a nine year old video on getting lithium from energizer batteries that i've linked in the video description.
So i won't go into it here.
I'm going to use two energizer batteries worth of lithium.
And there we go.
Now for our sodium hydroxide as well as our tertiary alcohol.
Let me hook up the bubbler.
Wait a minute, is that a dead fly in my bubbler?
Oh come on, why do bugs keep committing suicide into my apparatus?
Am i known in the insect world as the Dr. Kevorkian of depressed critters? Ugh.
Piece of s***
Anyway, now that i've cleaned the bubbler we can start.
I ramped up the internal temperature to just 125 C and held it there.
Unfortunately at this point my camera had a memory card error so i lost about 5 hours of video of watching the lithium dissolve and produce sodium.
Sorry about that. Here is the aftermath.
At least it worked though.
I can see a small amount of molten metal in there.
Lithium is solid at these temperatures so any liquid metal would have to be sodium or at the very least, a mixture of lithium and sodium.
So i let it cool and processed the resulting metal.
And there is our chunk of lithium and sodium metal alloy.
I didn't let it go far enough to completely convert into sodium as evidence by the continued hydrogen formation
but the fact that we're making sodium at this temperature means all the water had to be destroyed first.
And here is our cleaned flask.
And it looks great, no degradation.
Oh that white ring you're seeing that's not present in the original photo is actually there, but wet in the original photo so it didn't show up.
This new photo is not new damage.
It's also on the outside of the flask, so it can't have come from the reaction.
Bottom line, the reaction worked.
We have a way of starting the sodium production reaction by an alternate process that doesn't damage the glassware.
And it's very neighbor friendly, unlike the thermochemical dioxane process.
So we have solved the jumpstart problem.
Now i'm sure there are other better methods to jumpstart the reaction.
But this is simple, straightforward, and in the interests of time i'm going to move on.
We have almost fully conquered this project.
The next major problem i want to address is perhaps the most important of all: the alcohol catalyst.
While making these tertiary alcohols are well within the abilities of amateur chemist.
I want to find something even easier to get even if it's not as effective.
Now that we've optimized everything else, a less effective alcohol might actually be acceptable.
I'll address that in my next video.
Anyway, thanks for watching. We're getting ever closer to the end of our project.
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