Sciencemadness Discussion Board

Methanol production

Maja - 30-9-2008 at 10:54

Ok! I'm in need of methanol and can't get it ! Most of the suppliers needs permit to buy it(strange, because other much more toxic substances like pyridine, bromine etc etc etc...) can be bought without any problems! So how one would synthese methanol ? Also no OTC sources of methanol ! I have formaldehyde, but reducing that seems like a waste of time and money... Any ideas where to source or how to synthese CH3OH ?

Jor - 30-9-2008 at 11:23

where do you live? If in Europe, you can get methanol for sure, just ask me for the source.

Is it maybe possible to hydrogenate carbon monooxide?

ProChem - 30-9-2008 at 12:04

If you can find a methyl ester you can hydrolize it in caustic soda and distill off methanol. In fact a good experiment would be to take some scrap plexiglass and heat it in molten NaOH (under inert atmosphere) and see if methanol will distill off. The residue should be sodium methacrylate.

chemkid - 30-9-2008 at 13:24

HEET it is a common car product found even in convenience stores in the US. It is 99% methanol 1% proprietary ingredients. The proprietary can be distilled out with ease (so i hear). Make sure you don't get isoHEET which is isopropanol!

Chemkid

kalacrow - 1-10-2008 at 16:45

There are also some brands of denatured alcohol that are up to 40% methanol. Look at the MSDS for the cheap, generic kinds.

The other fraction would be ethanol and a bit of water.

Contrabasso - 24-10-2008 at 13:43

Search the world of bio-diesel they seem to get through a LOT of methanol with no access problems, just look on ebay for bio-diesel supplies.

I just don't know where all this impure glycerine is going to go ;)

Aqua_Fortis_100% - 24-10-2008 at 18:53

Quote:
Originally posted by ProChem
If you can find a methyl ester you can hydrolize it in caustic soda and distill off methanol. In fact a good experiment would be to take some scrap plexiglass and heat it in molten NaOH (under inert atmosphere) and see if methanol will distill off. The residue should be sodium methacrylate.


That is absolutely a good news to me.. If that actually works, it would be great since MeOH is not OTC (but at other hand you could buy anhydrous EtOH in almost any place here.. even so, that sucks for homemade biodiesel if you dont made the other reagents very anhydrous beforehand)..

I was originally thinking in methyl salicylate saponification then destillation..

Is there any other cheap/otc compound like plexiglas that one could, at least in theory, extract MeOH reacting with something?

[Edited on 24-10-2008 by Aqua_Fortis_100%]

S.C. Wack - 24-10-2008 at 19:30

Quote:
Originally posted by Aqua_Fortis_100%
Is there any other cheap/otc compound like plexiglas that one could, at least in theory, extract MeOH reacting with something?


Wood. Bonus: acetic acid and charcoal. A simple, clean, and fun weekend project for the kids. Quite a bit on this in the old industrial dictionaries, and IEC.

Aqua_Fortis_100% - 24-10-2008 at 20:03

Yeah..thanks for the help.
Indeed, wood is much cheaper, but that route can be very messy rendering several other impurities (acetic acid, aldehydes, ketones, etc and of course a lot of water).. But the worst part IMHO is the smoke/gas produced in that process it has a terrible smell..

There are some pics of my charcoal (retort method) I posted some time ago on apcforum (using another id):

http://i242.photobucket.com/albums/ff176/tnitrato/P9060023.j...
charcoal

http://i242.photobucket.com/albums/ff176/tnitrato/P9060024.j...
charcoal and wood

http://i242.photobucket.com/albums/ff176/tnitrato/P9060025.j...
improvised retorts (the small one I used for newspaper charcoal)

The foul smell forced me to turn down the can so that the smoke was intentionally directed to the heat source (flame) that burned it eliminating most of the smell.

Maybe distilling the aqueous products can give a reliable source of "100% homemade" MeOH, but separating it from the impurities can be even worse than hell..

I originally thought about using CaCl2 to remove the primary alcohol as a complex, like not_important advised on another thread, but Im not sure if the water from solution will 'suck back' the MeOH and avoid CaCl2 to 'attach' the alcohol..


[Edited on 25-10-2008 by Aqua_Fortis_100%]

[Edited on 25-10-2008 by Aqua_Fortis_100%]

kclo4 - 24-10-2008 at 20:27

Wow, I really like how you make charcoal!
personally, I've never looked into it since my yard has a ton of it for.. idiotic reasons, but I think its pretty cool how it heats itself by having the holes on the bottom!. I guess I'm impressed easily. :P

not_important - 24-10-2008 at 23:02

Quote:
Originally posted by Aqua_Fortis_100%
...
Maybe distilling the aqueous products can give a reliable source of "100% homemade" MeOH, but separating it from the impurities can be even worse than hell..

I originally thought about using CaCl2 to remove the primary alcohol as a complex, like not_important advised on another thread, but Im not sure if the water from solution will 'suck back' the MeOH and avoid CaCl2 to 'attach' the alcohol..


On a larger scale the gases are cooled to condense the valuable products and the non-condensible gases burned to help heat the retorts.

You need to get most of the water out first for the CaCl2 trick to work.

If you really wanted to work up the condensate, you'd follow the old method. Add Ca(OH)2 or CaCO3 to neutralise acids, if using CaCO3 adding some Ca(OH)2 after the CaCO3 has done it's job is useful as it hydrolyses esters, distill that to get everything boiling below 90C, then fractionate it to get MeOH and any acetone, dry that and fractionate. The residue in the pot from the 1st distillation will be water, calcium acetate, and higher boiling compounds. Concentrate until the acetate just starts to drop out of solution, dilute a bit, and filter through a pre-dampened fast paper (coffee filters will work) to remove much of the oily substances. Evaporate the filtrate to dryness, warm to 150 to 200 C to drive off volatile organics; then convert to acetic acid or crude acetone as wished.

Formatik - 25-10-2008 at 00:27

Distilling dry wood for methanol. Hmm, that would be an amateur feat, where according to the Dictionary of Chemistry by Watts, Vol.3, the watery distillate has about 1% MeOH. Watts also mentions almost very pure methanol is obtained by distilling wintergreen oil with NaOH or potash, and rectifying the distillate over CaO, where only a small odor from the oil goes over.

not_important - 25-10-2008 at 01:53

If you're meaning to get wintergreen oil from the plant, you'll find it's easier to use wood. Wintergreen ()Gaultheria is a cool climate shade plant, fairly slow growing; pyrolaceae likes it a bit warmer but still is a small not too quickly growing plant. Sweet birch might be better, but as it is a tree you'll likely have to wait a few years before you can start harvesting.

S.C. Wack - 25-10-2008 at 06:27

Donald Othmer apparently had little problem isolating an aqueous solution of methanol containing a little acetone, from his maple-filled retort 19" high and 15" in diameter. The calculated yield was higher than that which others had obtained previously.

[Edited on 25-10-2008 by S.C. Wack]

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kclo4 - 25-10-2008 at 12:01

Excuse me if this sounds ignorant, but what chemical in the wood decomposes into methanol? Cellulose and other carbohydrates would decompose into the carbon, and the lignin, which is mostly made of phenols I would imagine as distilling over as small nasty phenol compounds or something like that.

Perhaps you could find someone to send you methanol?
I can't Imagine that the sender or the receiver would be breaking any laws, from where you are, it isn't restricted is it? I know you said they need a license to sell it, but I don't know if that makes it restricted, hazmat or whatever else it can be placed under. :P

12AX7 - 25-10-2008 at 14:00

Carbohydrates in general. Lignins will give up aromatics and some aliphatic bits and pieces, but contribute well to charcoal because of aromatic stability and lignin's high overall carbon content (although charcoal is amorphous, it is chock full of rings of various sorts). You get all sorts of alcohols and aldehydes from the sugars, plus a bit of charcoal.

Fundamentally, you're driving off -OH units, which combine with nearby H's to form H2Os, and water is a primary product of destructive distillation, but what doesn't leave as H2O might leave with some carbon still stuck to it, and that's stuff like formaldahyde and methanol and longer chains, all the way up to the tars (which I'm guessing have a reasonable aromatic content) in lower yield.

Tim

not_important - 25-10-2008 at 23:11

lignin has methoxy groups, and those split off forming methanol; creosote also comes from lignin.

http://en.wikipedia.org/wiki/Image:LigninStructure.png

http://www.archive.org/details/2edwoodproductsdisdumeuoft
http://www.archive.org/details/woodproductsdist00dumerich


http://www.archive.org/details/technologyofwood00klaruoft

http://www.archive.org/details/chemicalmethodsf00veitrich