Transcription
I want to give a huge shout out to squarespace.com for sponsoring today's video. If you decide to recreate anything, it is at your own risk, and I do not accept the responsibility. Make sure you press the follow button on my Instagram, as if you were my ex pushing my [Music] buttons. I've got him in sights. Am I clear for the shot? You're clear. Over. Now, nitroethane is on the DEA's list, one chemical list, but it isn't illegal. It's just using, you know, a little bit of things. Though, some of the most common uses of nitroethane is a solvent for artificial polymers, dissolving cyano acry adhesives, and used as a reagent in various chemical syntheses. And just like nitromethane, this can be used as a fuel additive.
Now, to get the nitroethane, we could either do a synthesis or we could distill it from this product. Plastic craft has this product called Acrifix 1S 0117 pure that has nitroethane in it. It has ethyl formate with 30 to 60%, and it has nitroethane with 30 to 60% as well. I expect to get around 303 through 607 mL of ethyl formate and about 264 through 528 mL of nitroethane. And I could care less about whatever else I'm going to get.
Speaking of things I don't want, we do not want the ethyl acetate, buttin one all, or the two phoxy ethanol. Fractionally separating this shouldn't be too hard. The only problem is the nitroethane is very close to the boiling point of buttin one all. The boiling points are quite close to each other, so I'm a little worried. But buttin one all is only 1 to 5% of the solution. To start, all I did was just pour a random amount into a round bottom boiling flask. It did start to froth a little bit when I poured it in, and that made me a little nervous for the distillation. I didn't know if this was going to work very well, so I used around 2/3 of the bottle. God, this better work. I set it for a fractional distillation, and it was pretty much set to go. I turned on heating, and just a little bit after, you can see these really odd lines swirling around in the flask.
If you don't know what it is, then likely there's two things that are going on. Number one is convection currents, and even with multiple compounds, convection currents will still be present. As the solution heats, parts of it will warm up and rise, while the cooler parts sink, creating visible flow patterns or lines in the solution. The second one would be differences in the composition. So if our solution contains different compounds, which it does, with different boiling points or densities, likely we'll see lines or streaks where these components are separating or where one component is boiling and forming bubbles while the others are not yet. Also, if I'm wrong, forget everything I said. I also put boiling stones in there, so there's a point for nucleation. As a solution heats up, our distillation is starting to happen. Luckily, no frothing started to happen, and we could proceed forward with a fractional distillation.
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All right, it's time to lock back in. Ethyl formate should be coming over first at a boiling point of 54.3°C. The extra surface area in a fractional distillation column significantly enhances a separation process, leading to more efficient, effective, and pure separation of the components in our solution. The ethyl formate did start coming over at its boiling point, but then the temperature kind of rose to 62°C and stayed there for a little bit. I assume what's happening is something called boiling point elevation, and that's when the boiling point of a liquid increases because something else, like salts or another solvent, is dissolved in it. Basically, when you mix two things together, the mixture boils at a higher temperature than the pure liquid by itself. I decided to collect everything up to about 70 to 72°C and then switch the flask out so we can collect the ethyl acetate. Though, likely we're going to have a mixture of ethyl formate and ethyl acetate. I switched the flask out just so I could have a pretty pure product of the ethyl formate, and I really don't care about this middle fraction. I'm just going to pour this back into the bottle since it's going to be a mixture of things, and I'll just fractionally distill again.
I decided to collect this fraction all the way up to about 112°C. Once it was at that temperature, I decided to switch out the flask and start collecting the nitroethane. There is a huge gap between the ethyl acetate and nitroethane boiling point, so I thought it would be okay to start at this temperature. It did rise up to about 114 to 115°C and it stayed there for a while. The second this fraction hit 116°C was when I was going to remove the flask, since buttin one all's and nitroethane boiling points are so similar. I wanted to minimize the amount of buttin one all that comes into the nitroethane. Now, like I said before, it is only 1 to 5% of the buton one all, but it still matters. Frothing did start to increase as the distillation was coming to an end, however, it didn't present any issues and it stayed in the flask. Once the temperature reached 116°C, I switched the flask out just for a simple beaker. This should be the buttin one all, but likely there's a little bit of nitroethane in it. I'm also going to save this and put this back into the bottle.
Our first fraction that we collected all the way up to 70°C should be our ethyl formate. Ethyl formate can be pretty useful, and it has a characteristic smell of rum. The middle fraction is likely ethyl formate, ethyl acetate, and probably a little bit of nitroethane. Like I mentioned before, I'm going to pour this back in the bottle and re-fraction the distill. And our last fraction of nitroethane, which likely has a small impurity of buttin one all. I'm hoping that it's relatively pure and there's really not a lot in it, but I would really need a run under a GCMS or an NMR. I also weighed out how much ethyl formate I got in the end. I got about 120.82 g of ethyl formate. If this is pure, this would give us around 131.18 mL of ethyl formate. As for the nitroethane, I got 149.67 g. This equates, if pure, to about 142.27 mL of nitroethane. Nitroethane is generally a hard reagent to get, and this gives a possible solution to that problem. Like I mentioned previously, I'm going to pour the middle fraction back in the bottle as I know there's still a little bit of nitroethane in there. Now this was a trial to see if we could actually get it from this, and it does seem to be pretty successful. However, if you know a better way, please let me know in the comments, or if you have done this specifically, let me know exactly what temperature to collect each fraction at, and I will be very happy. And with that, have a good day. The video's done. Go do something else, and I'm going to go think about the Roman Empire.