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Author: Subject: pet ether/n-hexane from gasoline/petrol
Schmiddy
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[*] posted on 9-11-2019 at 07:23
pet ether/n-hexane from gasoline/petrol


hi

I recently had the desire to experiment with some petroleum ether so when looking for some hexane and wow is it expensive and hard to come by. I estimate that I would pay $150+ per L with S&H +DG fee.
That's not in the budget


so I did I little digging and found this


https://www.youtube.com/watch?v=UUYu4sEwdTw

so I ran down to the gas station,bought the lowest grade available and set up the glass ware. Did a couple runs through the vigreaux column and yeah I need a better column,these things suck,they work but are real touchy. It's needs to be distilled REAL slow.

I kept everything from 35 up to 68*C from several runs and now have about 1.3L of what I am calling raw petroleum ether.(correct me if that is wrong)

I plan to wash and further distil this as I want fraction from 40-68-ish*C.
I would like roughly a gallon(3.75-4L) of finished product.

Has anyone else done this and what has your experience been?
Any tips or hints?

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Pumukli
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[*] posted on 9-11-2019 at 08:53


Good luck with the distillation of petrol. It contains 15-20 different compounds (at least in my country), with close or overlapping boiling points, not to mention the possibility of azeotropes... You can try with a good column and very slow distillation, but...

If I were you I'd had visited a paint shop and 'd had bought something more promising, say "synthetic paint thinner" or something like that. According to the MSDS it contains fewer different compounds and MAY give better results. Check the fine print/msds on the glass/can before buying something with high aromatic content or an ester based thinner!

Another approach might be cold starter fluid. It contains diethyl-ether, yes, but sometimes it is a 50:50 mixture of ether and heptane. Again, check the MSDS first. Not as cheap as petrol or paint thinner, but definitely purer product and you may save the ether too, which is also a useful solvent to have.
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Schmiddy
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[*] posted on 9-11-2019 at 09:44




where I live you need a company license to buy anything other than latex paint and deck stain(consumer grade stuff).


I'm not after pure n-hexane and am happy with the mix(for the time being)
I was after pet.ether and was gonna settle on ordering some n-hexane until I saw the price.

My basic goals are a solvent that boils above 40* below 70* and contains no benzene or unsaturated compounds and is immiscible with water.

although I will possibly be distilling starting fluid for ether in the next couple weeks,God willing,that's diethyl ether and not what I'm currently after.

also the cost of it, a 300g can of starter fluid is over $10 while a liter of gas is less than a dollar and contains a good 25-40% of what I'm after.

of all my OTC sources for a pet. ether/hexane gasoline seemed the highest yielding, cheapest and is working out good so far.

Gasoline and oil in general, is a fascinating mix and although I live in major oil producing region I never really appreciated undecomposed wood juice until now
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[*] posted on 9-11-2019 at 09:49


correction: I stated starter fluid was over $10 for 300g aerosol can and it is $7 per can

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[*] posted on 9-11-2019 at 17:14


Quote: Originally posted by Schmiddy  


where I live you need a company license to buy anything other than latex paint and deck stain(consumer grade stuff).


I'm not after pure n-hexane and am happy with the mix(for the time being)
I was after pet.ether and was gonna settle on ordering some n-hexane until I saw the price.

My basic goals are a solvent that boils above 40* below 70* and contains no benzene or unsaturated compounds and is immiscible with water.

although I will possibly be distilling starting fluid for ether in the next couple weeks,God willing,that's diethyl ether and not what I'm currently after.

also the cost of it, a 300g can of starter fluid is over $10 while a liter of gas is less than a dollar and contains a good 25-40% of what I'm after.

of all my OTC sources for a pet. ether/hexane gasoline seemed the highest yielding, cheapest and is working out good so far.

Gasoline and oil in general, is a fascinating mix and although I live in major oil producing region I never really appreciated undecomposed wood juice until now


Unfortunately, gasoline contains a large percentage of unsaturated alkenes (maybe up to 40%) so loves to react with stuff. I found this out the hard way, so maybe try searching a bit harder for other solvents.
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[*] posted on 9-11-2019 at 20:05


Quote: Originally posted by Deathunter88  
Quote: Originally posted by Schmiddy  


where I live you need a company license to buy anything other than latex paint and deck stain(consumer grade stuff).


I'm not after pure n-hexane and am happy with the mix(for the time being)
I was after pet.ether and was gonna settle on ordering some n-hexane until I saw the price.

My basic goals are a solvent that boils above 40* below 70* and contains no benzene or unsaturated compounds and is immiscible with water.

although I will possibly be distilling starting fluid for ether in the next couple weeks,God willing,that's diethyl ether and not what I'm currently after.

also the cost of it, a 300g can of starter fluid is over $10 while a liter of gas is less than a dollar and contains a good 25-40% of what I'm after.

of all my OTC sources for a pet. ether/hexane gasoline seemed the highest yielding, cheapest and is working out good so far.

Gasoline and oil in general, is a fascinating mix and although I live in major oil producing region I never really appreciated undecomposed wood juice until now


Unfortunately, gasoline contains a large percentage of unsaturated alkenes (maybe up to 40%) so loves to react with stuff. I found this out the hard way, so maybe try searching a bit harder for other solvents.


I was going by the wiki article and it says that 10% H2SO4 wash deals with that.
from wiki:
Most of the unsaturated hydrocarbons may be removed by shaking two or three times with 10% of the volume of concentrated sulfuric acid; vigorous shaking is then continued with successive portions of a concentrated solution of potassium permanganate in 10% sulfuric acid until the color of the permanganate remains unchanged. The solvent is then thoroughly washed with sodium carbonate solution and then with water, dried over anhydrous calcium chloride, and distilled. If required perfectly dry, it can be allowed to stand over sodium wire, or calcium hydride.[6]

https://en.wikipedia.org/wiki/Petroleum_ether

If I was in correct in this please advise.
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[*] posted on 10-11-2019 at 05:11


Quote: Originally posted by Schmiddy  

where I live you need a company license to buy anything other than latex paint and deck stain(consumer grade stuff).


Where do you live? This sounds drastic...
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[*] posted on 10-11-2019 at 07:07


Quote: Originally posted by Heptylene  
Quote: Originally posted by Schmiddy  

where I live you need a company license to buy anything other than latex paint and deck stain(consumer grade stuff).


Where do you live? This sounds drastic...


normal for many places in North America now. if you want commercial or industrial grade products you need a business license

long gone are the days when you could pick up chemicals at the drug store and dynamite at the hardware store.

I have to show my drivers license to buy stump remover or disinfectant now.



[Edited on 10-11-2019 by Schmiddy]
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[*] posted on 10-11-2019 at 10:17


I too am very curious as to your state because it's nothing like that here. I can't believe stump remover is like that there! I didn't realize just how easy I had it. Sure, I can't get 5 gallons of methanol delivered to my doorstep from an industrial ebay seller or chemical supply house, but it's simple to file some registration paperwork and legitimize yourself for most chemistry purchases here.

If you can distill a suitable fraction from gasoline then more power to you! Starting from basics can be more fun, and the end results more appreciable. I haven't dealt with pet ether either because of its price but I'll definitely keep an eye on your results.
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[*] posted on 10-11-2019 at 12:17


Quote: Originally posted by Schmiddy  
Quote: Originally posted by Deathunter88  
Quote: Originally posted by Schmiddy  


where I live you need a company license to buy anything other than latex paint and deck stain(consumer grade stuff).


I'm not after pure n-hexane and am happy with the mix(for the time being)
I was after pet.ether and was gonna settle on ordering some n-hexane until I saw the price.

My basic goals are a solvent that boils above 40* below 70* and contains no benzene or unsaturated compounds and is immiscible with water.

although I will possibly be distilling starting fluid for ether in the next couple weeks,God willing,that's diethyl ether and not what I'm currently after.

also the cost of it, a 300g can of starter fluid is over $10 while a liter of gas is less than a dollar and contains a good 25-40% of what I'm after.

of all my OTC sources for a pet. ether/hexane gasoline seemed the highest yielding, cheapest and is working out good so far.

Gasoline and oil in general, is a fascinating mix and although I live in major oil producing region I never really appreciated undecomposed wood juice until now


Unfortunately, gasoline contains a large percentage of unsaturated alkenes (maybe up to 40%) so loves to react with stuff. I found this out the hard way, so maybe try searching a bit harder for other solvents.


I was going by the wiki article and it says that 10% H2SO4 wash deals with that.
from wiki:
Most of the unsaturated hydrocarbons may be removed by shaking two or three times with 10% of the volume of concentrated sulfuric acid; vigorous shaking is then continued with successive portions of a concentrated solution of potassium permanganate in 10% sulfuric acid until the color of the permanganate remains unchanged. The solvent is then thoroughly washed with sodium carbonate solution and then with water, dried over anhydrous calcium chloride, and distilled. If required perfectly dry, it can be allowed to stand over sodium wire, or calcium hydride.[6]

https://en.wikipedia.org/wiki/Petroleum_ether

If I was in correct in this please advise.


Doesn't work like that in real life, trust me I tried... Dilute sulfuric acid doesn't do much, and anything more concentrated causes polymerization of the alkenes into a black tar and no way you're separating out anything useful from that.
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[*] posted on 10-11-2019 at 12:20


Quote: Originally posted by Schmiddy  
Quote: Originally posted by Heptylene  
Quote: Originally posted by Schmiddy  

where I live you need a company license to buy anything other than latex paint and deck stain(consumer grade stuff).


Where do you live? This sounds drastic...


normal for many places in North America now. if you want commercial or industrial grade products you need a business license

long gone are the days when you could pick up chemicals at the drug store and dynamite at the hardware store.

I have to show my drivers license to buy stump remover or disinfectant now.



[Edited on 10-11-2019 by Schmiddy]


it's the same story in China for a few years now. First they required the equivalent of your SSN for buying 95% alcohol, now they don't sell anything above 75%. You can be arrested for 15 days for possession of paint thinner or any other flammable liquid. It's ridiculous.
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[*] posted on 10-11-2019 at 14:05


Extrations and Ire did a nice couple of videos distilling gasoline. You might take a look and learn from his experience.
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[*] posted on 10-11-2019 at 14:13


Quote: Originally posted by j_sum1  
Extrations and Ire did a nice couple of videos distilling gasoline. You might take a look and learn from his experience.


that's exactly what he linked in the first post





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S.C. Wack
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[*] posted on 10-11-2019 at 15:11


You omit the KMnO4 then say it doesn't work? Distillation of gasoline is organic chemistry? If there are light alkenes, they will not harm cannabis extracting (which I suspect is what you and several other new accounts of last few years are really up to) if they can be removed later.



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Schmiddy
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[*] posted on 10-11-2019 at 15:43


Yes the ask for photo ID now for Potassium nitrate whether in the form of stump remover or as fertilizer from the hydroponic/garden store. I tried both.

They don't however give two shits about Calcium Nitrate or sodium bicarbonate,so figure it out.

30%H2O2 again requires photo ID but 3% doesn't.

well this project is working out so far,I'm up to a liter of washed and dried pet.ether

This is good enough for what I need it it(which does involve plant extractions,cannabis among them now that it's legal)

I'm out of raw petrol for further refining so this project is on hold until I get more funds for gasoline.

extractions and ire did do a fine job of giving me a road map,I set my glass up differently than him and I'm uninterested in any fraction over hexane/68*C right now so the tails are being store for later use ,of which I have not determined.

I may try to film a future distillation and washing as pet ether is something that is often referred to in literature but is tough for amateurs to obtain.

I'm pretty sure chemist 100yrs ago obtained their pet.ether exactly the same way I am getting it,DIY from gasoline
I'm thankful I didn't have to blow my own glass(although a metal distiller would work)

It fumes rather impressively and the vapor pressure is enough when slightly shaken to pop off the solid glass stoppers.
That amuses me thoroughly

since the price of gas has come down even more since I started I may also try for a clean fraction of n-hexane as it seemed to be a large cut in the last few runs.
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