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Old 12-31-2006, 05:58 PM
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It works !!!

Finally got the time to finish making my methanol recovery still. It worked great!!!

Question??? for Fabman (or any of you Guru's out there that are using a hot water tank as a still)

When do you know when you have all the methanol out of the glycerol???

What I did is I started with a sample run of 20 gal. of glycerol. As advertised it started to drip at about 150* over a period time it slowed so I raised the temperature over time, till I was at about 190*. Out of that 20 gal. of glycerol that I started with I got about 7 gal of crystal clear methanol but it was still coming out when I had to shut down for the night. I drained the tank and I only got about 10 gal of residual glycerol. But it seemed that it would have still continued to pour if I would not have shut down and continued with the 190* temperatures but I was afraid that I would start to evaporate water that might be in the glycerol.

My question is when do you know you have all the methanol out? And about what amount can I expect to recover in gallons verses gallons of glycerol which I started with?
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Old 12-31-2006, 07:54 PM
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Originally Posted by Gun-Driver
Finally got the time to finish making my methanol recovery still. It worked great!!!

Question??? for Fabman (or any of you Guru's out there that are using a hot water tank as a still)

When do you know when you have all the methanol out of the glycerol???

What I did is I started with a sample run of 20 gal. of glycerol. As advertised it started to drip at about 150* over a period time it slowed so I raised the temperature over time, till I was at about 190*. Out of that 20 gal. of glycerol that I started with I got about 7 gal of crystal clear methanol but it was still coming out when I had to shut down for the night. I drained the tank and I only got about 10 gal of residual glycerol. But it seemed that it would have still continued to pour if I would not have shut down and continued with the 190* temperatures but I was afraid that I would start to evaporate water that might be in the glycerol.

My question is when do you know you have all the methanol out? And about what amount can I expect to recover in gallons verses gallons of glycerol which I started with?
Good for you! 190 deg F is just perfect, when it starts to drip slower and slower its done. As long as you keep it below 200 deg you won't get any water.

I recover about 40-45 percent from my glycerol, and another 5-8 percent from my Bio.
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Old 01-01-2007, 08:23 PM
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Fabman,
The recovered methanol looked crystal clear in a small glass, but when I filled up a gallon jar it had a just a little bit of a yellowish/green tint. I compared it to new methanol and the new stuff was clear. Is that discoloration normal or is there something up with the recovered methanol? I haven't had a chance to track down a hydrometer to test it. Just wondering if yours was the same color.

Last edited by Gun-Driver; 01-01-2007 at 08:26 PM.
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Old 01-01-2007, 08:56 PM
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Quote:
Originally Posted by Gun-Driver
Fabman,
The recovered methanol looked crystal clear in a small glass, but when I filled up a gallon jar it had a just a little bit of a yellowish/green tint. I compared it to new methanol and the new stuff was clear. Is that discoloration normal or is there something up with the recovered methanol? I haven't had a chance to track down a hydrometer to test it. Just wondering if yours was the same color.
I've noticed the same "tint" to mine also, but my Hydrometer says 95-98 percent. I think it's carrying over a small fraction of KOH.

The new system I'm testing now shows 99 proof, with no tint at all. The good thing is you'll be able to convert your system over to the new system easily! It should require less energy [ only have to heat to 150 deg ], and produce a more refined Methanol. And a LOT faster............
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Old 01-01-2007, 09:05 PM
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Great let me know when you have completed the plans and testing.
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Old 01-02-2007, 06:39 PM
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Fabman,
Finally got a hydrometer, was getting 92% @ 60* which is the temperature it said to test at. How can I get a higher percentage or is 92% ok? And how long does it take you to yield 10 gallons of recovered methanol. It seemed to take a long time for me to get that amount. I'm going to make some changes to my system to see if I can speed the time up some.
And what do you do with the left over byproduct after you recover the methanol. I poured the waste from yesterday's first batch in a couple of cubes I had laying around. Checked it today and it was a very stiff paste. So I cut the top off the cube and I could hardly scoop it out. What do you do with this? How and what can I use it for? My wife wants to make soap from it, have you ever done that.
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Old 01-02-2007, 07:11 PM
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Quote:
Originally Posted by Gun-Driver
Fabman,
Finally got a hydrometer, was getting 92% @ 60* which is the temperature it said to test at. How can I get a higher percentage or is 92% ok? And how long does it take you to yield 10 gallons of recovered methanol. It seemed to take a long time for me to get that amount. I'm going to make some changes to my system to see if I can speed the time up some.
And what do you do with the left over byproduct after you recover the methanol. I poured the waste from yesterday's first batch in a couple of cubes I had laying around. Checked it today and it was a very stiff paste. So I cut the top off the cube and I could hardly scoop it out. What do you do with this? How and what can I use it for? My wife wants to make soap from it, have you ever done that.
Sounds like your temp may be "spiking" higher than 190, try and keep it around 175 deg. It should still work however.

It took me FOREVER to get it all with my old still, that's why I went to a vacuum system. The vacuum system cut the time by about 1/3, but was still to slow.

The new system will process about 20 gallons of glycerol per MINUIT! Much faster, and a whole lot less hassle!!!

If you are using KOH, you can heat the recovered glycerin to 150 deg, mix with an equal amount of HOT water and use it as fertilizer. If you are using NaOH, you can do the same, but it is a weed killer!

Yes I've made soap out of it too. NaOH based glycerin will make a "hard" bar soap. KOH based glycerin will make a great liquid hand cleaner. I've got a recipe for glycerol soap, It's at the shop and I won't be there for the next couple of days, but I will find it and post it here.
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Last edited by fabmandelux; 01-02-2007 at 07:14 PM.
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Old 01-02-2007, 08:47 PM
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Gun-Driver
Distillation is a well accepted method of seperating a mixture into its components as long as the components each has a different boiling point.
The boiling point of methanol is 64.7 degrees C (148.5 degrees F). Water boils at 100 degrees C (212 de3grees F). Glycerol's boiling point is 290 degrees C (554 degrees F) and the boiling point of KOH is over 1300 degrees C. Biodiesel is a mixture of very similar methal-alkyl esters all of which have boiling points well over that of water.

The point is all you have to do is get the temp over 150 degtrees F and the MeOH will boil off. Lower temps will require longer boil off times.
There will always be a small amount of water vapor included and probably even a very small amount of glycerol, it has to do with vapor pressure and it's why you wont get to 100% by distillation alone. You can use drying agents or a molecular sieve to improve the purity but you won't get to 100% with out spending huge amounts of money.

Fabs new method sounds very interesting. Hope he shares it soon.
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Old 01-03-2007, 07:36 AM
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Can I still use this recovered methanol at 92%? I was thinking of mixing it in with my new methanol, would that be ok?
Second question; If I used a larger diameter pipe it my condenser to allow more volume to travel through (as long as I cn cool it sufficiently) would that speed up the recovery. It took around six hours to recover 10 gallons.
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Old 01-03-2007, 07:44 AM
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Originally Posted by Gun-Driver
Can I still use this recovered methanol at 92%? I was thinking of mixing it in with my new methanol, would that be ok?
Second question; If I used a larger diameter pipe it my condenser to allow more volume to travel through (as long as I cn cool it sufficiently) would that speed up the recovery. It took around six hours to recover 10 gallons.
You should be able to use it just the way it is, but you can also mix it with "new" methanol.

Using a larger condensing coil will not speed up the process [ been there, tried that!]
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Old 01-03-2007, 03:20 PM
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I would add one caveat.
Using your recovered MeOH with 8% unknown contaminant means you are dealing with an unknown ph.
I would be tempted to titrate a few batches until I felt comfortable with the quantities of reagents. Then I would spot check from time to time.
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Old 01-04-2007, 08:21 AM
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Do you mean to use the recovered methanol to do the titrate to see if I get a different reading? I titrate for every batch, so what I may do is a titrate test with new methanol and a test on the same oil with the recovered methanol and see what the difference is. I'll be out of town on business for the next six days when I get back home I'll pass along how the test's went.

Thanks guys for all the info and help!!
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Old 01-04-2007, 09:43 PM
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What you should do is "blankl titration" of your new MeOH before you process a batch with it after processing do the same with a sample of the recovered MeOH and compare how many drops of your reference solution it took to neutralize each.
The closer the results the less the chance of unhappy results when using recovered MeOH to process..
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Old 01-05-2007, 08:21 PM
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Gun-Driver

Fabs new method sounds very interesting. Hope he shares it soon.
I'm working on it..............Have to get the patent application back from the attorney. Can't put it in the public domain until that's done. I will post the plans here for free, just trying to protect my self.
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Old 01-06-2007, 09:32 PM
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I'm working on it..............Have to get the patent application back from the attorney. Can't put it in the public domain until that's done. I will post the plans here for free, just trying to protect my self.

Yup ya gotta do that for sure!!
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Old 01-06-2007, 09:32 PM
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