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Junk_Enginerd
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[*] posted on 7-6-2020 at 04:02
Simplest "power solvent" synthesis?


Sorry about the vague "power solvent" term. I just don't know the technical term. What I mean is something in the chloroform, MEK, THF class, which dissolves a lot of plastics that acetone and ethyl acetate won't. I do a lot of tinkering and building, and for example 3D printed PLA would be great if I had a solvent for, and I know all of the above mentioned will dissolve PLA. I also enjoy experimenting with plastics and solvents in general, so a powerful general purpose solvent would be great. Nylon is something I've wanted a solvent for as well.

I have synthesized chloroform, which went well and worked well, but the quantity you get using acetone and sodium/calcium hypochlorite is pretty impractical. I'm looking for a process which could yield me at least 500 ml or so of solvent without excessive work and less than, say roughly $40 in materials.

A lot of the solvents somewhat easily synthesized require starting materials that I can't procure. Methanol is one seemingly very handy starting point, but finding pure methanol seems quite impossible. The solvents I have mentioned are also next to impossible to find anywhere for a civilian. Im in Sweden, so I don't have the same possibilites for off the shelf stuff. Ideally the synthesis wouldn't require more exotic substances than acetone, alcohol, chlorine sources and other mostly basic chemicals. I do have some quantity of the most common acids and/or ways to synthesize them, if that helps.

Heating, distilling, vacuum and other basic processes are no problem.

Any suggestions?

[Edited on 7-6-2020 by Junk_Enginerd]
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Pumukli
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[*] posted on 7-6-2020 at 04:22


Dioxane comes to mind, but it is unhealthy (carcinogene). There are synth descriptions of the compound here in SM.

Maybe dimethyl-dioxane isomer mix would also be possible starting from propylene-glycol, I don't know.

How "omni solvent" would dioxane be I'm not sure either. But synthesis-wise it would give you the most "splash" for the buck I think.
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[*] posted on 7-6-2020 at 07:19


ethyl acetate? esterification of ethanol with acetic acid




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monolithic
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[*] posted on 7-6-2020 at 07:54


I think chloroform is the simplest and easiest solvent synthesis. If you buy bleach for pools it's usually 10% concentration compared to 4-6% for household bleach, which helps cut down on volume. I run the reaction directly in the plastic jug: chill to -20 C, add half your acetone, let react until temp rises to 25 C, chill again to -20 C, add second half of your acetone, then let react and sit at room temperature for 2 hours. Decant/separate/dry/distill. A three gallon pack at Home Depot is about $10 which yields 300-350 ml of chloroform.

I have made 1,4-dioxane from ethylene glycol and it's more time consuming because it involves multiple distillations, stirrings, etc. The dehydration step is a pain in the ass to clean up and it stinks. You also have to take precautions because it can form explosive peroxides. You can read my simple write-up here: https://www.sciencemadness.org/whisper/viewthread.php?tid=84...
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[*] posted on 7-6-2020 at 08:16


If you use really big flasks and very good stirring, you can simply make larger amounts of chloroform by Ca(OCl)2 in stirred suspension.
You need about a 10-20l flasks due to the horrible foaming and hard to control exothermia, but then you can make over 250-500ml of chloroform at once in a single sitting.
At least that is what I would say based on my own experience with 100g of the hypochlorite and acetone in a 2l flask which I ran three times with around 60ml of chloroform(I think).

I run the whole thing in a distillation setup and use the exothermia that sets in with carefully adjusted dropping in of the acetone to the heavily stirred mixture.
It has the reaction set in with a certain time delay, so you really have to be careful.
But when it has set in, you just keep the reaction going with your addition rate and the resulting chloroform distills out, and then only needs to be redistilled once again.
Very well working for when you need a bit larger amounts.
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[*] posted on 7-6-2020 at 12:20


You can try synthesising GBL. It is said to be very aggresive for plastics and it's easily obtainable from GABA (you can find it in supplement shops) by Sandmeyer reaction. Neither it is carcinogenic and unhealthy, you can even drink it :D :D. But keep in mind that it's probably illegal in your country and its second destiny is being a drug.
Maybe you can try synthesising different lactones by the same route, or maybe some keto acids.
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[*] posted on 7-6-2020 at 13:16


N-methylpyrrolidone should be as useful as GBL without the accompanied legal implications, but with likewise solvent capabilities.
After all, it is in graffiti remover, and that involves sometimes dozens of layers which are essentially a thick piece of plastic of mixed composition.
Those are what I would call I power solvent.

If everything else fails: maybe you need to discover the mythical alchemical solvent called alkahest?
Here: https://en.wikipedia.org/wiki/Alkahest
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[*] posted on 7-6-2020 at 13:45




Quote: Originally posted by Pumukli  
Dioxane comes to mind, but it is unhealthy (carcinogene). There are synth descriptions of the compound here in SM.

Maybe dimethyl-dioxane isomer mix would also be possible starting from propylene-glycol, I don't know.

How "omni solvent" would dioxane be I'm not sure either. But synthesis-wise it would give you the most "splash" for the buck I think.


Dioxane seems strong enough for my purposes from what I can gather. Do you have any idea how carcinogenic it is? Like, occupational hazard or acute hazard carcinogenic...?


Quote: Originally posted by Ubya  
ethyl acetate? esterification of ethanol with acetic acid


Ethyl acetate is very much like acetone. It's a decent solvent, but useless for PLA, PET, Nylon, etc.

Quote: Originally posted by monolithic  
I think chloroform is the simplest and easiest solvent synthesis. If you buy bleach for pools it's usually 10% concentration compared to 4-6% for household bleach, which helps cut down on volume. I run the reaction directly in the plastic jug: chill to -20 C, add half your acetone, let react until temp rises to 25 C, chill again to -20 C, add second half of your acetone, then let react and sit at room temperature for 2 hours. Decant/separate/dry/distill. A three gallon pack at Home Depot is about $10 which yields 300-350 ml of chloroform.

I have made 1,4-dioxane from ethylene glycol and it's more time consuming because it involves multiple distillations, stirrings, etc. The dehydration step is a pain in the ass to clean up and it stinks. You also have to take precautions because it can form explosive peroxides. You can read my simple write-up here: https://www.sciencemadness.org/whisper/viewthread.php?tid=84...


Hm. That's annoying to hear. Though I suppose getting it to work reliably with calcium hypochlorite would require less pricey chlorine. I sure can't get 3 gallons of pool chlorine for $10. I'd expect to pay at least 3-4 times that. I can get 1 kg of calcium hypochlorite for about $15 though, and that's a lot more chlorine...
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[*] posted on 7-6-2020 at 13:50


Then buy large flasks cheap from china and you can run it like I outlined with Ca(OCl)2 and acetone.
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[*] posted on 7-6-2020 at 15:31


Dioxane is probably less carcinogenic than chloroform, if that's your point of comparison. Both can become dangerous on storage, with chloroform producing phosgene and dioxane forming explosive peroxides. Chloroform has low flammability; dioxane has a lower explosive limit (LEL) of 2% at STP.

Acetonitrile can also be produced relatively easily by refluxing acetamide over alumina. It is not known to be carcinogenic. It is flammable with LEL 4.2% at STP.

http://www.sciencemadness.org/talk/viewthread.php?tid=11137&...

I don't know if acetonitrile or dioxane will dissolve the particular substance of interest in this case, though. It may be wiser to simply find a source of DCM, which dissolves everything :p




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 7-6-2020 at 15:52


I second the suggestion of finding DCM. If you’re in the US, it’s currently being phased out of consumer products, but remaining stock of DCM paint stripper still seems to be available at hardware stores. All you need to do with it is distill it to remove the proprietary polymer gunk, wash with water to remove the methanol, dry, and distill once more. It’s a lot less expensive and much higher yielding than making chloroform, and a little less time consuming too. Maybe you’ll even find it on sale! Temporary silver linings of chemical restrictions...



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[*] posted on 7-6-2020 at 22:27


Isopropylnitrite should be capable to dissolve even grease used for joints (did not try it by myself, just saw it in one video). But it is quite dangerous, it decreases blood pressure, it has quite low boiling point etc...



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[*] posted on 10-6-2020 at 13:54


Quote: Originally posted by clearly_not_atara  
Dioxane is probably less carcinogenic than chloroform, if that's your point of comparison. Both can become dangerous on storage, with chloroform producing phosgene and dioxane forming explosive peroxides.


Chloroform is really stable, if you store it under light for xxx years it probably will give 0.0000 ppb of phosgene... not dangerous at all. But it is very Narcotic ! Use it only in a well ventilated area.

Concerning dioxane there is a tiny tiny risk of peroxide. The only solvent that can make peroxide is diisopropylether, then THF. And even with these solvent the risk of peroxides formation is a kind of myth.

When I was at the university we gathered all the worst conditions for peroxide formation :
- non stabilized THF
- only 50ml with a lot of air in a 1l bottle
- directly in the sunlight
- let for 6 month
and... NEgative to the peroxide test....

This myth comes from the 50's when people did peroxidations in THF and then concentrated the solvent to the rotavapor and BOOM !
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[*] posted on 10-6-2020 at 16:59


Re peroxides: is the use of copper in ether bottles so relatively unknown actually?
Nobody mentions that, and everyone I recommend that too seems to be deeply surprised that this is such a well working method to prevent peroxide formation in advance.
I don't get it, copper is easy to get, cheap, and it works.
Simply something like a piece of thick cable, granules, or whatever else is on hand... the surface is roughened for better results and then the copper is simply left all the time in the bottle.
Not much is needed too... and throught at least 3 bottles of DIPE, I've used the same copper rod and never had any peroxides in there(although, used the bottles in around six months up anyways...).

But there are enough online informations that confirm the usefulness of copper as a preventive measure against peroxides!
It won't remove them, as some seemingly think... but why even letting it come so far, with this metal preventing them even forming in the first place?
Its much easier to put some copper into your ether than it is to test for, in turn destroy its peroxides and purify the solvent again, all the time you could have spared...
And all that just because you missed putting whatever copper items you have around in there...?
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[*] posted on 10-6-2020 at 17:39


I didnt know that, interesting information.

Like I said before, this is very hard to make ether peroxide. Try to make a test by pouring H2O2 or tBuOOH and you will see the difference with and without copper rod.
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[*] posted on 10-6-2020 at 18:47


Quote: Originally posted by Texium (zts16)  
I second the suggestion of finding DCM. If you’re in the US, it’s currently being phased out of consumer products, but remaining stock of DCM paint stripper still seems to be available at hardware stores.


No the environmentalists killed off DCM completely. You can't even buy it off Ebay anymore. You used to be able to get gallons of it at Lowes or Home Depot under different brands but the environmentalist pointed to the horrible horrible stat of like 2 or 3 people dying from it over 40 years and that was enough to kill it off (those 2 or 3 people used gallons of it to strip paint in a completely enclosed room).

You can now get ethyl acetate at hardware stores now though because of them phasing out MEK. The "MEK Substitute" at Home Depot is just ethyl acetate.
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[*] posted on 11-6-2020 at 05:10


Guys, the OP is from Sweden. A very "green" country or so they speak... I doubt if he/she was able to find DCM easily in that country. (Although DCM is just one "miracle solvent", yes.)
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[*] posted on 11-6-2020 at 22:55


Im also in Sweden and you can buy 25L pails of sodium hypochlorite (bleach) at the hardware stores.
It has 12-14% concentration and thats much higher than the bleach at other stores.
Just remember that the % of sodium hypochlorite will go down with time in storage so its best used pretty fast.
You can also order DCM on ebay. Its not common but pops up sometimes.
I just ordered 10L DCM and some Acetic Anhydride on ebay.
Also, if you order from within EU it wont pass customs and that can be useful if ordering some more restricted chemicals.
When ordering stuff the whole EU is like a country and items from outside EU is passing customs but after that it can be sent anywhere within EU without passing customs again.
Methanol can be ordered from UK if you cant find it some other place, no customs from UK either.
I also order Sulfuric & phosphorous acid from a german company without problems.
Sulfuric acid is harder to get than most things here.
In Sweden its hard to get chemicals but if you know where and how almost anything can be ordered.
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[*] posted on 12-6-2020 at 04:14


Then the OP should check e.g. Limac Science and order solvents from them. They are within EU and carry some nice to have things, e.g. various solvents. It is much better to have these basic things from a trusthworthy seller in known quality than to try to synthetize them. More exotic stuff, yes, go for preparations, but preparing solvents and such... I'm glad I can buy acetone by the liter and not forced to synthesis. But for each of his own.
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[*] posted on 12-6-2020 at 11:09


Quote: Originally posted by Pumukli  
Guys, the OP is from Sweden. A very "green" country or so they speak... I doubt if he/she was able to find DCM easily in that country. (Although DCM is just one "miracle solvent", yes.)


Indeed. And even if it wasn't for that, just the fact that it's a small country greatly limits options. And EU does too. Booring.

Quote: Originally posted by Mateo_swe  
Im also in Sweden and you can buy 25L pails of sodium hypochlorite (bleach) at the hardware stores.
It has 12-14% concentration and thats much higher than the bleach at other stores.
Just remember that the % of sodium hypochlorite will go down with time in storage so its best used pretty fast.
You can also order DCM on ebay. Its not common but pops up sometimes.
I just ordered 10L DCM and some Acetic Anhydride on ebay.
Also, if you order from within EU it wont pass customs and that can be useful if ordering some more restricted chemicals.
When ordering stuff the whole EU is like a country and items from outside EU is passing customs but after that it can be sent anywhere within EU without passing customs again.
Methanol can be ordered from UK if you cant find it some other place, no customs from UK either.
I also order Sulfuric & phosphorous acid from a german company without problems.
Sulfuric acid is harder to get than most things here.
In Sweden its hard to get chemicals but if you know where and how almost anything can be ordered.


I think if I'm gonna make chloroform I'll do it from calcium hypochlorite instead. Way higher concentration, so no need to handle so much bulk. It's pretty cheap too. I'll be distilling it anyway, so all the calcium crud won't even really matter.

Good tip on UK. I'll look that up.

Sulfuric acid is, surprisingly, no issue for me. I have access to plenty of batteries to harvest, and concentrating it is ridiculously simple. I've actually got a good stash of all of the most common acids. But yeah, trying to buy sulfuric acid is a shitty experience. Though I think the permit is quite simple and relatively cheap to get, and then it's super simple.
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[*] posted on 12-6-2020 at 14:40


Off but important those, who order a lot from the UK. Brexit is going to happen in January. There is no sign from the British gov. they want a deal. It will result WTO rule trade between the EU and the UK. All goods will have to be declared going in or out.
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[*] posted on 14-6-2020 at 05:46


That is true, so ordering stuff from UK to other EU without passing customs (and other way around too) might end when UK leaves EU permanently in about 6-7 months something.
Maybe i should order some stuff while its still possible.
UK and EU might make some trade agreement for the future but it seems like UK will leave EU at beginning of 2021.
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[*] posted on 14-6-2020 at 06:56


This got me curious. I live in the EU.
Does no customs really mean it's safe to order whatever? I've been needing some more restricted stuff lately, mostly iodine/KI, though I would absolutely jump at the chance to safely acquire reagents like acetic anhydride and NaBH4 or solvents like DCM, DMSO and perhaps even THF for future use.

So far I've just been synthesizing chloroform from ~20% NaClO but I would much rather replace that with DCM if it were practical.


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[*] posted on 14-6-2020 at 07:00


In CZ you can buy DMSO without any problems. But I don't know how easy you get it in other countries.



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