Does this actually make sense?

Rabidreject

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Hi guys,
I guess I have two questions I guess but they are both relating to the same subject - sodium ethyl sulfate.
Okay so first things first - does this synthesis make sense?

I know that mixing sulphuric acid and azeotropic 98% ethanol to make sulfonic acid and from there basically basify, evaporate and the re-x to rid it of the impurities.
There are loads of papers on this and I’m certain it works, however, I only have 85% sulphuric acid.
Am I going to have to do the scary distillation of sulfuric acid in order for that to work? There is water used later in the experiment but from what I understand when you are first mixing the sulfuric acid and ethanol you are making sulfonic acid which I believe is a reversible rxn depending on water content.
is it going to be too much water to just use it as it is?

obviously if the first synthesis is actually correct - it’s easier and less dangerous!

just thought I’d take advantage of y’all expertise instead of blindly following some pootube guy!

thanks guys!
 

Frit Buchner

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Are you asking if there is too much water in 85% H²SO⁴? No, there's no water in it if thats you question. Very specific reason.
 

Rabidreject

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Are you asking if there is too much water in 85% H²SO⁴? No, there's no water in it if thats you question. Very specific reason.
Frit BuchnerI guess I was primarily asking people to watch that YouTube video and tell me if the science is sound because it looks like ‘bro science’ to me.
iv only seen this done successfully (as in the synth of sodium ethyl sulfate) and backed up by papers by mixing conc. sulphuric acid with ethanol and then basifying (an acid/ base RXN) which is reversable dependent on water content (I believe - I need to write it up in my own lab book and break it down into suitable steps so I don’t f it up - rather than keep popping up a pootube video)
I DO read papers and patents but I find I learn much quicker and it sticks in my head a lot better and just clicks when I see it done. Sorry for so many replies - as I said I’m a little scared to start without having distilled my H2SO4 - I don’t trust myself with nearly 400c boiling pure acid in my mantle or frankly anywhere near me!
By the way, I love your username!
 

Rabidreject

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Are you asking if there is too much water in 85% H²SO⁴? No, there's no water in it if thats you question. Very specific reason.
Frit BuchnerOh also, I asked the guy to go through the science of it and give me the equation but he hasn’t yet responded. In the other (sulphuric acid) video I watched yesterday - as I say I’ll need to watch it again and make notes BUT he goes through the equations on a white board sliced into his videos. Really useful guy. I’m surprised they’ve not banned his channel actually but hey ho
 

Rabidreject

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Yeah I guess that’s one of my questions - the latter half. I was wondering if the first synth makes sense - refluxing as pure ethanol as you can get with sodium bisulphate and then I believe he filtered it out and proceeded as he did in the other work up after adding sulphuric to the ethanol. I just don’t see how it could make sense…
 

Rabidreject

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So I guess, will the 85% sulphuric acid (no matter what it’s mixed with - it would help if you could tell me why it wouldn’t be water, would that react?) be strong enough to work to make the sulfonic acid needed for the next step - I guess it should do, if it is mixed with other stuff surely once it’s reacted I can re-x. I know I’ll lose yield but I just don’t trust that first reaction I pointed to which is why I named the thread so…I just wanted to add that as a secondary question regarding the 85% sulphuric acid instead of 95%…you’ve got me curious - I’ll use google to see why it wouldn’t be mixed with water - there was me thinking I might be able to freeze precip the water out! I assume it’s too strong of an acid to use anything like a mol sieve or silica balls? I just don’t fancy boiling sulphuric acid if I can get away with using what is already there - it’s for growing consumable plants so I can’t see it being ANYWHERE near as horrible stuff, as Is in the drain cleaner you see people distil it from. This stuff is slightly thick and clear in colour….so what do you think? As well as answering why it wouldn’t be mixed with water? This is vital for me to get started - well I guess it’s not but it’s a pricey enough mistake to go straight in with everything! It’s nice that it’s an exothermic rxn too, I prefer them over having to add heat.
I guess I’ll find out later as I plan on doing it in small / probably micro scale to you people lol talking 1g of each here. See if it goes exothermic for a start….I been thinking to see if it eats through tissue paper as that seems to be the test they use on YouTube to see if it’s pure lol
Man I learn way more WATCHING someone do something and unfortunately none of it gets checked. So sometimes someone can think they are making something - like I think may be the case in that first you tube link, when it’s just ‘bro science’ instead of actual correctly worked out science.
 

Rabidreject

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I guess I’ll try it both ways! I have both the equipment and reagents so why not. I’m going to use denatured ethanol though - for the most part. I do have a little XXX ethanol (as I call it because I need to distill 3x to get it to 95-98% and dry it with moll seives)
 
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