Started methanol recovery on 500 gallons of Glycerin ive been storing up for a year yesterday.

The temp wet up pretty slowly before anything started happening. Took about 5 hours to hit 155. At 160 she started flowing. Collected untill about midnight. The temp stayed around 160-164 the entire time. So far i've collected 60 gallons of methanol. I believe there is more that will come out, so im going to continue distilling over a second day.

Just hit 110 Gallons recovered and still temps are only at 185.

Cool!
What kind of still setup? Is your glycerin contaminated with water? If so what is your recovered meth purity?

Jon

If you do the 5% prewash, at 185 degrees you are only getting 85 to 90% pure methanol and that would be with a good reflux setup.

it would also depend on if 185 was the head temp or the pot temp. head temp purity will be low.
I run my pot temp to around 200F.
make sure the pump can handle the temps otherwise you destroy the shaft seal

-dkenny

Well, The total count is 150 gallons. My temps come from the pot and are now at 198. Its still flowing at a steady rate although the flow has cut to about 1/2 of what it was.

I dont have any exact data on the glycerin. I do 2 stage, with between 16 and 24% methanol...depending on how long ago it was made. Yes i do a prewash but its not ever more than 2% max.

As for the purity of the methanol...who knows. I do have a hyrometer but have not yet tested it. I assume the first 60 gallons is the purest...

Edit: My still is a 20 foot long super plumbers delight. 1" copper crimped alternating every 2 inches housed in a 3" PVC sleeve.

After the last post I got another 12 gallons out Which brings the total to 162 gallons...Its down to a drip now and I'm pretty much tired of the distillation of this batch...Its taking FOREVER!!

Temps hit 208F

I plan on making a bunch of soap out of this so I wanted to get as much methanol out as I possibly could.

You should put a thermometer into the vapors at the head of the condensor so you know what you're getting out. That's the relevant temp that tells you what you're actually distilling off, not the pot temp...

Though about doing that, but it was after i had already started...My next upgrade though

Just strap a thermometer probe of some sort to the beginnning of the column and wrap a large amount of insulation around it to make it a bit closer to being an accurate reading.

(note: there are TONS of remote thermometers in the right ranges for what we're doing at Lowes these days, including the digital barbeque/cooking thermometer variety and also a really cheap thermocouple-based one in the multimeter section of "electrical")

What im planning on doing is installing a thermocouple and wire it into my existing PID control. That way the PID will be able to control the exact temp at the condenser for the highest purity.

What kind of reflux capability do you have?

Wow, 162 gallons from 500 gallons of glycerine by product. Thats something like 32% yield. That is way higher than we have ever achieved.
I would take a look at your purity to see what kind of stuff you are making.
We use 20% methanol in our BD reaction so we start out with less to begin with.
I am very curious as to the purity of what you have made.
DD

Fabricator,

Being new to the methanol recovery, what do you define as "reflux capability"?

DD,

Didn't get a chance to check the purity yesterday. I was rushing to get the Gly out of my processor before it cooled and hardened. It appears to have separated over night into liquid and gel. The liquid came out first about 120 gallons, then the gel came out about 200 gallons. Id say that the majority of this Gly was made at 18% methanol.

Did your fuel pass 3/27? If it is low conversion, you'll also have more methanol left over than if it were high conversion.

Yes, My fuel always passes 3/27

Let me see if I can find a pic.

Ok, that is my still, the 4" pipe you see sticking out of the top is filled with marbles, my thermocouple is in the base of the 4" pipe, and I usually have it set at around 160 degrees, so all the marbles in the column are always at 160 degrees so the methanol vapor will flow up through the marbles and be unaffected and exit through the condenser, water vapor however will condense on the marbles and fall back down the column and into the pot, this is refered to as reflux.

Nice!
Judging by the size of it you are using this strictly for the glycerol?
What are you using for the condenser and the coolant for it?
It looks like you have an immersion heater in the top of the tank? If so is that to heat up your reflux column? Are you heating the glycerol with an immersion heater? Vacuum involved?...
I now 20 questions write!?
How is your purity... was it worth the effort?

Thanks,
Jon

JCBIO,
if you can wire the PIDs as an 'AND' setup.
in other words. both pids (pot and head) require heat for the heat to turn on. this give the greater safety margin to the setup. i used to have this until i lost my pids and replaced them with different ones and an SSR instead of relays.
I now have a switch that controls which pid controls the temp..this is not a good setup, i'm going to change this, since the pot temp has not upper limit..the pot temp will go as has a need to drive the head temp to its limit if it can!! not good..

for faster results inject air into the system. if the PID controlling the head temp si doing its job the purity will stay high. I run my head temp at 152F. this is at the top of the reflux column. purity is 99%.. I used this for doing a 27/3 and the results compared to using the yellow isoheat methanol.

-dkenny