Everyone is on the right track with the column temp. The best way to separate water from the methanol [besides rerunning with another distillation process] is leaving the reactor into a good 2 stage designed reflux column that controls the head temp.

The best design out there is scalable and used in large Ethanol operations, the Charles 803 design. Typical output is 95% or higher purity only. Anything below that falls out the bottom of the column or stillage port to a separate tank. I had one, now another member on here has it.. I have the plans and will try to scan them in, or you can buy them online too for like $35 US.

-Ken

quote:

I have the plans and will try to scan them in.

That would be great!

I'm fabricating my 2nd processor that is now domed top and bottom from a 66gal HWH.
I'm trying to learn all the bells and whistles to make a fast and effective setup.
I will be demething the bio inside the reactor, so I can go to settling, and then drywash.

Saw your videos today, very good examples. Thanks for sharing.

Brian

a 3C swing in temp is WAY too large.. I have a 1 degree F swing. 3C is almost 6F..

refluxing helps.. consider using a loose packed column.

I have read the large diameters help

they get 95% out of ethanol distillation..WOW that great I think 96% is max for ethanol.

fyi ethanol and methanol differ in this aspect. its possible to higher purity using distillation with methanol but not ethanol. there's a technical term here, but I cannot spell it.. ..ethanol and water like each too much.

-dkenny

miscible I think is the word you are looking for

quote:

Originally posted by dkenny:

they get 95% out of ethanol distillation..WOW that great I think 96% is max for ethanol.

fyi ethanol and methanol differ in this aspect. its possible to higher purity using distillation with methanol but not ethanol. there's a technical term here, but I cannot spell it.. ..ethanol and water like each too much.

-dkenny

Personally I prefer a good 60-70% ethanol, not bad straight and blends very well with many things..


An interesting side fact is you can run a 80-90% pure Ethanol in a internal combustion engine without problems. But when you blend it with gasoline to make E85 or whatever, the water will fall out unless it was 99% or better to start. Anyone know if that's the same with Methanol?

3A or 4A zeolite is widely used drying Ethanol before blending. I would imagine it works as well on Methanol. Thanks Rdrake100 for the memory jog. One advantage to this chemical is, you can quickly regenerate it on a gas grill. The Q&D I've been playing with for BD drying takes a long time to air dry.

-Ken

While searching online for a digital copy of the 803 reflux plans I found another site with MANY great still plans.

http://www.homedistiller.org/

Look under "Equipment" then "Making A Still" for plenty of great reflux column designs. Some of them are cool variations on the plumbers delight design.

Also found mail archive link off the Biofuel mailing list where JTF pulled the Charles 803 design from the site stating it didn't perform as stated, and problems from people who purchased and never received the plans. It's JTF, so go figure...

Soon as I find a drafting size flatbed scanner, I'll donate my copy for review.

-Ken

here are some photos of ours, we consistently get 98-99% pure methanol. Just a simple 55 gallon drum setup with reflux column, column is filled with 2 boxes of copper scrub pads and the rest with marbles. Temp control is at the top of the column using standard thermostat. We no longer use the pump to recirculate.

http://www.biodieselpictures.com/viewtopic.php?t=614

Nice design with the air cooled condenser, I've looked at those pix before :-) Farmer is using a similar setup with a modified AC unit for cooling and also reported good results. But you know that since we both were at his shop, just realized that...

I need to get you in touch with my partner on the soap biz, he is just getting started into it and we've got 500 gallons of NaOH Glycerin right now. If ya need any extra let me know, I'll gladly bring you some next time I head that way. I did some extended camping [2 years] just over the hill from ya in UBE.. Nice area of PA.

-Ken

quote:

Originally posted by dkenny:
its possible to higher purity using distillation with methanol but not ethanol. there's a technical term here, but I cannot spell it.. ..ethanol and water like each too much.
-dkenny

The word you are thinking of is Azeotrope This limits the distillation of ethanol by simple distillation to about 96%/ 192 Proof grain alcahol.
It is my understanding that the places that produce 100% fuel ethanol usually get the last 4% of water out by running it through a molecular sieve.
Another method is to add a chemical such as benzine which "Breaks" the azeotrope. The down side is that benzene is a poison so you would not want to use it in your martini.

And you are correct, methanol and water do not form an Azeotrope so you should be able to achieve 99% or better purity using simple distillation

quote:

Originally posted by Kenr34:
Nice design with the air cooled condenser, I've looked at those pix before :-) Farmer is using a similar setup with a modified AC unit for cooling and also reported good results. But you know that since we both were at his shop, just realized that...

I need to get you in touch with my partner on the soap biz, he is just getting started into it and we've got 500 gallons of NaOH Glycerin right now. If ya need any extra let me know, I'll gladly bring you some next time I head that way. I did some extended camping [2 years] just over the hill from ya in UBE.. Nice area of PA.

-Ken

Last time I was at Dickinson college he was using a plumbers delight, that was last fall.

We're plenty good on NAOH glycerin for now but thanks! I'm sitting on about 100 gallons of de-methed stuff right now and get about another 10 gallons each month. Our still is doing a real good job and our bar soap is much firmer now than when we started, the de-methed glycerin gets so hard I have to use a small shovel to get it out of the drum we store it in.

I purchased 10 pounds of 3A zeolite to see how well it would purify my 90% methanol. It came in two 5 pound metal tins, so i poured my methanol into the container just enough to cover it.I put the tin inside a bucket with a lid, as it gets quite hot, and gives off mucho vapours.

I left it overnight, and then inspected for results. I had put just over 2 litres of methanol into the zeolite, and most was adsorbed, and what could be recovered was only marginally improved. A bit of a disappointment. However, sometime later when i was transferring some contaminated methanol, i noticed an oily residue on the bottom of the carboy, so my guess is that the methanol was somehow bonded with oil, and thus adsorbed - evidently zeolite very readily adsorbs hydrocarbons.

I have been advised to be careful in regenerating the zeolite...first air dry it to drive off any methanol, then it can be put in an oven at 100C.

azeotrope is the word or is it hydrscopic {alchohol is very hydrscopic to moisture} dkenny [here's a technical term here, but I cannot spell it.. Frown ..ethanol and water like each too much.]

Hello all it's been a while sence I'v been here. As one of you sail the simplest way is overlooked. Well I have your solution to all your distilling problems. Any one want to know what it is ? I distill about 45 to 50 gallons at a time with purity between 95 to 100% any one want to know more as to how this is done? You will laugh at this bet it works and it too simple. Thats all Ill say for now get back to me if your interested.

do tell!

Not yet but it is so simple, I dont even check on my still but once a day. I run 45 to 50 gallons of glis in it, usely get from 14 to 17 gallons of methnol that is 97% or better in purity. It takes about 48 hours to retrieve the meth. My question is would any one pay for this info or should I patten it, produce it and sell it. With every thing you need to build this still it cost about $225.00
You dont even have to weld any thing but you do have to solider a couple of joints.

If your not going to detail the process, why bother posting what you have figured out? Keep it to yourself and market it then. Otherwise, spill the beans.

I wouldn't pay for it.
Thanks anyway.

Your right I wouldn't pay either. I used a 55 gal drumb,insulated, 1" drain on the bottom and air port in the bottom with about 2 lbs of air injection. Removable lid with 2" bung, 4' copper tower full of marbleswith a gage in the top, 1/8" copper coil in a water jacket. cold in the bottom hot out the top the 3/4" bung has a tempature gage in it. Now for the best part you want to know how I heat it right. Get back at me you will be shocked, the suspense has you new !

[QUOTE]Originally posted by mason1956:
.
Now for the best part you want to know how I heat it right. Get back at me you will be shocked

____________________________________________________________________________________________________



Lemme guess, you have Rush Limbaugh and James Carvel under the drum blowing hot air?


Come on man, let it out of the jar, Mason.

Now that might work, LOL 1500 watt heat band on wraped around the bottom of the drumd, no controls, no shutoffs, takes about 45 hours and your done. any questions ? it works Great!