AdamAlden
I have a theory about life, the universe and everything.
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Registered: 18-3-2016
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ether recycling and storage
just wondering if anyone has a good process for recycling and storing / purifying this solvent without it blowing up. after reading a lot about it i
decided i cannot work with it till i fully understand it. to understand it i need someone to tell me what to do to purify it and what not. cause i
read it degrades into explosive compounds over time how could i neutralize these compounds and then distill it before use (after drying)
im honestly not trolling im actually afraid of ether i made it a few times with i swear i think its sodium nitrate and sulfuric acid but the yeild is
pretty small but to be honest if its purest quality is from a proce oh wait thats nitric acid i did that too i need pure ethanol and some other shit
to make ether i forget though. i followed a video on nurdrages youtube channel back in the day to make the ether. it was funny i think they are my
cousins or some shit but they were only little i was in the garage making ether and they came in i immediately told them to get out they asked what
are you doing i said... im making a bomb lolololol they ran off
I am a buttmeister
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teodor
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I'm not an expert here, but what I basically do:
1. Test for peroxides with sodium ferrothiocyanate reagent. I did some posts about it here: https://www.sciencemadness.org/talk/viewthread.php?tid=15793...
2. Remove peroxides if present with ferrous sulfate. Vogel has a procedure.
3. Distill if necessary. Use only a long spiral condenser (Graham) and cold ethanl (let say, -20C). There is still no guarantee there is no lost on
this stage. Be careful, can catch fire. (The autoignition temperature is just 160C)
4. Dry over CaCl2.
5. If you need super dry put a sodium wire. I modified a tobacco press bought on amazon for the purpose of making it. Also was following Vogel.
Update: as a field of experiments, if you have very dirty ether, you can try
making and breaking various etherates. But practically, if you can manage distillation without considerable loss making of you own ether could be more
economical.
[Edited on 27-3-2025 by teodor]
[Edited on 27-3-2025 by teodor]
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MrDoctor
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so, with radical scavengers such as BHT, or perhaps hydroquinone? you can pretty much keep the ether peroxide at bay. what is tricky is storing it,
but there are some tricks i have found.
On aliexpress there are these things called "leak proof essential oil bottles", its an aluminum cannister with a very firm push-insert plug of sorts,
followed by a PP screw cap, its the same bottle youll find high-end or just especially noxious epoxy/fiberglass resins come in. this combination
provides a pressure-tight seal preventing ether from escaping.
if you buy 10 at a time or more they can get rather cheap, i think i paid no more than $3 or 4ea for the 250ml ones.
Otherwise, a close second is cheap "fuel bottles" which i dont really understand, their application is camping, and they connect to gas stoves, but,
they are meant to contain gasoline? certainly not butane/LPG, i dont know. but they have a screw cap with a rudimentary gasket and while they leak
enough vapor to smell, they barely lose a gram of mass per month if you use teflon tape to improve the seal. ether and DCM however soften the cap so
you want to be rather conservative with how often you use it. i dont use them anymore except for long term storage of my DCM.
Ether is very difficult to keep contained, and if even a trace is escaping you pretty much cannot refrigerate it at all then, through various
mechanisms, it causes refrigerators to blow up.
what i have heard is the ether condenses on icy coils, where it oxidizes and can form ether peroxide, eventually resulting in combustion, though its
the fumes that fill the fridge that actually do the damage, the ether peroxide on the dry evaporator coil ice just potentially provides some form of
ignition eventually, assuming this fridge doesnt have the thermostat inside the cooling compartment. especially small bar fridges, will have the
thermostat inside, resulting in there being a periodic arc as the contacts connect.
My workaround has been to simply keep my bottles which barely leak as it is, inside a 12v peltier cooler with no fans or anything, the lid is super
leaky and moisture is constantly flushing any residues out as it dissolves into condensation, which can drain away. its inefficient but i dont lose
any tangible amount of ether even during 40C days, and i can keep it outside of the house too. though the place i keep it could be defined as a barn i
suppose, or car shed, which is why the sweet-water that dribbles on the ground doesnt make a smell. indoors in an enclosed space it could be a
problem. During winter the fridge doesnt need to run at all so i leave it open and off, but spring and summer, i think my bottles would explode.
without cooling i had the issue of ether just freely boiling if i opened the bottle.
Note: ether diffuses rapidly through teflon and silicone, the more of either you use, like, the thicker it is, the worse diffusive leakeage becomes.
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Osmiridium
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First of all you really tried to produce ether from NITRATE, sulfuric acid and ethanol? I hope you didn't distill that shit off the mixture?
What you will produce is not diethyl ether but ethyl nitrate and that is unstable and explosive as hell. This would be a really stupid idea.
A few other remarks:
It's never good to be afraid of things in chemistry. This can lead to accidents too. But of course it's crucial to inform yourself about any dangers
and properties of the substances you intend to work with. What you apparently did not. If you are afraid and don't know what you are doing, leave it
alone.
And I would really never make jokes about making a bomb. You know, people talk. You can have the best intentions and do nothing wrong, still in our
paranoid society if the wrong people hear something you can get in serious trouble. Then it's no joke anymore.
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MrDoctor
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Quote: Originally posted by Osmiridium  | First of all you really tried to produce ether from NITRATE, sulfuric acid and ethanol? I hope you didn't distill that shit off the mixture?
What you will produce is not diethyl ether but ethyl nitrate and that is unstable and explosive as hell. This would be a really stupid idea.
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From the looks of it they used speech to text and forgot to cut the nitrate part out. Nurdrage afaik never made ethyl nitrate, but has done ether.
Also, just mentioning this but if you have access to iodine tincture, the fact you have a strong purple solution (as iodine not povidone iodine) means
you have enough iodine for a colormetric test for peroxides. off hand i forget what the test was i think starch and iodine? or perhaps it was a weak
acid and iodide salt, since the peroxide would oxidize the colorless iodide/hydroiodic acid into dark iodine again. in any case the iodine is the only
one tricky to get for some in this very easy and versatile set of colormetric tests, but all this requires is a visual color change which even
milligrams in tincture gets you easily, and afaik tincture is available almost universally.
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Osmiridium
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| Quote: Originally posted by MrDoctor | | Quote: Originally posted by Osmiridium | First of all you really tried to produce ether from NITRATE, sulfuric acid and ethanol? I hope you didn't distill that shit off the mixture?
What you will produce is not diethyl ether but ethyl nitrate and that is unstable and explosive as hell. This would be a really stupid idea.
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From the looks of it they used speech to text and forgot to cut the nitrate part out. Nurdrage afaik never made ethyl nitrate, but has done ether.
Also, just mentioning this but if you have access to iodine tincture, the fact you have a strong purple solution (as iodine not povidone iodine) means
you have enough iodine for a colormetric test for peroxides. off hand i forget what the test was i think starch and iodine? or perhaps it was a weak
acid and iodide salt, since the peroxide would oxidize the colorless iodide/hydroiodic acid into dark iodine again. in any case the iodine is the only
one tricky to get for some in this very easy and versatile set of colormetric tests, but all this requires is a visual color change which even
milligrams in tincture gets you easily, and afaik tincture is available almost universally.
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You would use iodide and starch. Iodide is oxidized to iodine and that forms a deep blue complex with starch and indicates presence of an oxidizing
agent. This test is so sensitive that it can be used to quantitatively determine oxidizer concentrations through titration.
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eyeemplus
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Ether purfication
See the attached graphic
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MrDoctor
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oh i need to try that, my ether contains something, and if aldehydes for example dont just distill out normally, or wash out with water, i would
assume that means they are quite difficult to remove by any means of seperation.
How reliable would permanganate be for this? like to totally eliminate, if that fails ill try that copper-zinc stuff. Some of my ether comes through
the reactor with this strong odor attached that no amount of distillation can cure, nor soaking with acid, base, charcoal or just water. i thought it
was some polymer of some kind which is why it could have virtually identical physical properties, based on something i read somewhere
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