distilling chemicals for meth
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Cheapskate (Newbee ) 7/24/00 11:32 AM
Re: Distilling Chemicals for Meth [Post#: 32624 ]
Obtaining Restricted Solvents in California
Folks in California that want to do research into chemistry have a special problem that is not shared inmost other states: Toluene and DCM are just not available outside of a chemical supply. Yes, I know thereare a few stores scattered around that have it, but they're few and far between. If one doesn't want to getrecorded in the DEA's list of nasty people, one has to travel to other states or use mail order suppliers.Traveling works pretty well, but takes time and money. Mail order still gets you on a list and you have topay huge shipping costs for chemicals. Fortunately, with a little work, DCM and Toluene can be isolatedfrom common paint stripper.
At the local big homeowner store there's a product called Strip Ease. The contents lists MethyleneChloride, Toluene, Acetone, Methanol as well as some kind of polymer thickener. All of these are usefulsolvents to the clandestine chemists, but how to separate them and get rid of the polymer?
If you try to filter this stuff the polymer will clog up anything. Even vacuum filtering for hours doesn't help.You can't let this stuff set and see a separation of the solvents, the mix makes them miscible in eachother. You can distill them, but distilling a gallon of this stuff is a real pain using the normal flasks andaccessories available to a clandestine chemist's budget. Fortunately, there is a solution!
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First, give up on recovering the Methanol and Acetone. The Acetone isn't worth the work, it's easilyavailable in gallon containers at the same store. The Methanol is worth the work, but almost impossible toseparate from the Acetone without really special efforts. Methanol can be obtained from the auto parts storeas a product called, "Heet" or something similar.
Go to the local really big discount general department store and get a large stainless steel pot. You wantone of at least 3 gallons capacity, bigger if you want to do more. The pot has to have a good lid and it'sbest if the lid has a single knob on the top that is screwed in place. I got a 5-gallon pot for boiling malt forbeer for US$23. When you get this home, remove the knob and replace it with a glass fitting that will fit yourdistilling setup. I had a 24/40 female fitting (actually three, from a flask that I broke) available. Yes, you willhave to make the hole bigger; a round file works great for this. If you don't have a glass fitting available, justsilicone seal the distillation adapter directly into the top. You'll eventually break a flask and have the fittingavailable.
Now you have a multi-gallon distilling flask. Pour a gallon can of the paint stripper into the pot. Rinse thegallon can with a gallon of water and put the water into the pot. You now have two gallons of stuff in the pot,so put the lid on and duct tape it around the lid so there are no air leaks. This pot doesn't have to withstandpressure, you're going to do this without vacuum, it just has to contain the vapors while it boils.
Now set up to distill. Use electric heat, flames will probably explode the solvents and we need all theclandestine chemists we can get. The mix will start to boil around 40C the boiling point of DCM. Actuallyhere's the list of items that you'll get out of the distillation:
Dichloromethane, Methylene chloride, DCM, bp. 39.8, density, 1.3255Toluene, bp. 110.6, density 0.867Acetone, bp. 56.2, density 0.7857Methanol, bp 64.6, density 0.791Water, bp 100, density 1
As you can see, it should distill over as first DCM, followed by Acetone, then Methanol, Water, then lastlyToluene, but it doesn't happen this way. There are several azeotropes formed and the water will tend to takethem all over together. This is a very complex distillation, so don't try to figure it out, just get the good stuffand leave behind the polymer. The whole purpose of this first distillation is to separate the liquids and leavethe polymer behind.
Fluid will come over beginning around 40C and will continue as the temperature starts to rise. Empty thereceiving flask as necessary into a jar and notice that there will be some separation of the fluids in the jaras they set. Stop the distillation at 90C. Yes, there will be some toluene and water left in the pot, but if you
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as they set. Stop the distillation at 90C. Yes, there will be some toluene and water left in the pot, but if yougo above this temperature the polymer will melt and start to distill over. While you're cleaning the distillingpot, let the fluids set and separate, there will be two layers. One of the layers is Methanol, Acetone andWater, the other is DCM and Toluene. Yes, there is some mixing of the solvents still, but the next stepswill take care of most of this.
You want to wash the DCM-Toluene mix with lots of water. Just pour water in, stir it up real good then pourthe water off. There may be some problems here, if the mix is just right, the water layer will be on top andeasier to remove, but if the mix is proportioned differently, the water layer will be on the bottom. This iswhere a separatory funnel comes in, to remove the bottom layer. You can tell which layer is which bypouring water in and watching where it goes. Wash the mix thoroughly at least 3 times with an equalvolume of water to DCM-Toluene. This will remove the Acetone and Methanol as it dissolves in the waterand is poured away. You'll lose a small amount of DCM to this process, but it's not much. DCM onlydissolves in water to 1 part in 50.
You're now left with a solution of DCM and Toluene. The boiling points are far enough apart so thatdistillation is easy, but use a fractionating column anyway. There's still enough water in there to make thedistinction between solvents hard to tell during distillation and it's a lot easier to manage the process if thedistillation slows down as the DCM is distilled out before the Toluene comes over.
Depending on the volume of fluids, use a distilling flask or the pot and distill away. The DCM will come overfirst starting around 38C to 42C. Change flasks at this point and continue distilling until the temperaturerises over 100C and then change flasks to collect the Toluene. There will be a rather quick jump from 101Cto 110C as the Toluene comes over. The distilling flask or pot will be left with a small layer of green crapthat is useless, discard it. You may be able to recover more DCM from the solvent mix that comes overbetween 42C and 100C, but you decide if it's worth the effort to distill this small amount of fluid again, Inever do.
The DCM will be somewhat cloudy with a few drops of water floating around in it, separate the water and drythe DCM by pouring through a couple of inches of anhydrous magnesium sulfate. Remember that DCM willdissolve 1 part in 50 to water, well the reverse is true also, so there's some water there. The Toluene will beclear and pretty with no visible water (unless some dropped in from the setup), but dry it throughmagnesium sulfate to remove the water that is invisibly hiding in there. To test that this really worked,Toluene is flammable and DCM isn't. Put a drop of the Toluene on something and apply a match, it'll burn. Ifyou do the same to the DCM, it won't burn. Isn't chemistry wonderful?
This technique will work for several brands of paint stripper, even the one with the nasty orange goo in it.Enjoy.
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Subject Posted by Posted on
Distilling Chemicals for Meth Damien_Thorne 7/24/00 01:39 AM
Re: Distilling Chemicals for Meth Unobtainium 7/24/00 02:12 AM
Re: Distilling Chemicals for Meth Cheapskate 7/24/00 11:32 AM
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