Transcription
[Music] Hello everyone, and welcome back. So I thought I would try to prepare ethyl sulphonic acid. I have in this flask around 160 milliliters of ethanol. You're going to add it to the flask. [Music]
And in this graduated cylinder here, I have 80 milliliters of concentrated sulfuric acid. This was distilled from drain cleaner and it's pretty clean. I was very careful about the distillation, as you've seen in a previous video, and I have tested it a little bit, and it seems to be just at 98%, so what with a small margin of error for my measurements. So I'm going to add this next, and it's going to produce quite a bit of heat, so I'm going to have to add it rather slowly. In fact, I'll move the camera closer so you can see it as it happens.
I also need to drop in a stir bar. I'm going to use my dirtiest stir bar because the sulfuric acid ought to clean it up a little bit in the process. That's a just surface staining; there's no appreciable [Music] impurities that will be imparted by that. So I have my sulfuric acid and this graduated cylinder, and I'm gonna add it very slowly with stirring. So let me turn on my machine here. Okay, so I've got stirring going, maybe a little too much to the splashing; get to a good stir rate. Okay, that looks good to me. All right, now we'll add very slowly through the funnel. [Music] See the boiling it's causing; trying to keep that out of your control as I'm adding. I don't want it to start refluxing until I have to convince Iran, but this is going to get it pretty hot. [Music]
This process is called a Fischer esterification or a Starification, if I could talk, I could probably explain it better. So I'm gonna continue adding my sulfuric acid slowly until I've got it all in. Oh boy, it's been rather hot. [Music] As the concentration of sulfuric acid begins to rise in here, you'll notice that the boiling has calmed down some, and that is because the boiling point now it is much higher in this mixture because sulfuric acid on its own has a very high boiling point; ethanol boiling point being in the 70s, 70 Celsius somewhere around there, you know, it's relatively low in comparison, but the mixture of the two creates a boiling point that's much higher than that of ethanol. As this heats up from being mixed that concentrated sulfuric acid increases, so does the boiling point, and it stops being able to reach the boiling point in the mixture. And at a certain point, there's a lot of a lot of points in that sentence, but you get what I'm trying to say. [Music]
This is why you got to be careful with sulfuric acid; already eating at my gloves. I've been I've changed them the first time I measured this out with the it's real fast, real fast stuff; it'll sneak up on you. Fortunately, it hadn't gone all the way through yet, but my fingers are kind of warm. It's crazy how fast that happens; notice my fingers getting warm, and I was like, well, it's probably on my gloves. That's no good stuff; it's an incredibly strong oxidizer; it will eat through gloves in short order. What we're all in now, and we'll connect the condenser, and then I'll turn the heating on. And this preparation that I was reading was saying to reflux for 2 to 3 hours. So this is going to heat for a while, and I'm gonna let it reflux for 2 to 3 hours, and then I'm gonna come back and take it off the heat and let it cool down, and then we'll continue the procedure to the finish, to the to the end of it, where we will be neutralizing the solution and converting—well, I'll explain it when we get there.
So this is a round 2 here; the first time I did this didn't go so well. The flask actually had boiled over into my heating mantle and caused a short-circuit, killing my heating mantle. And actually, I have ordered the part that I need to fix it, and this is gonna be its whole thing, you know, to repair it; the triac was blown out. In any case, since I do have a little hot plate and this oil bath and everything else, I was able to repeat the experiment again, being more careful this time. And now in this flask, I have what should be ethyl sulphonic acid and a small amount of ethanol, a small amount of sulfuric acid, and some water obviously. But what's really interesting to me is I've done this experiment once or twice before, and you know, I wasn't using as pure sulfuric acid or as dry ethanol, and I never got it to change color like this. I mean, this is a really very drastic difference from when it started, so I believe this to be a much more positive result than I've had in the past.
So in any case, one thing I would like to try to do is convert it into a salt. So I thought I would try to convert it to the sodium salt, which could be sodium ethyl sulfate. So what I need to do now is I need to pour the reaction mixture into a beaker and start neutralizing with calcium carbonate. That produces the calcium ethyl sulfate and calcium sulfate, and calcium sulfate is not soluble in water, whereas calcium ethyl sulfate is. So you'll get rid of the excess acid in the sulfate salt of calcium and keep the calcium salt of ethyl sulphonic acid in solution. That was a mouthful; hopefully, it makes sense. So I'm going to start doing that. Once we've done that, that we can work the calcium salt through the sodium salt using sodium carbonate, and we've got our end product at that point. Anywho, I'm gonna get started. [Music] You [Music] [Music]
Well, it looks like I'm gonna have to use some sodium carbonate after all; I ran out of potassium carbonate. This makes this a little bit more challenging, but should be okay. [Music] [Music] You may be wondering why I'm using gravity filtration here, and the cheap reason is that my vacuum pump died, and I am really or not, not into the idea, you know, the little manual pump thing that I got; these uh this guy these things work, but it's a huge pain in the butt to use; it's just it's it makes your hands exhausting. [Music] [Music] You