Methanol recovery?
Hi everyone.
We are now processing our third 3 liter mini batch of biodiesel. Yippee! We are becoming more familiar with the process with each batch. We ordered two kilos of KOH from Fischer Scientific, along with two lab aprons and a box of lab gloves. However, I forgot to order phenophelien as we want to go with it for titration instead of the pH meter method we began with. Now that I write this I see I have two questions. What are the different pH values that phenophelien, pheno-red and what is the other one called? Bromo- blue? Anyway, Fishersci.com seemed a bit pricey on the phenophelien. Anyone know of a good source for these? Second, with these small (3L) test batches we are using HEET and the cost is way too much, even at $.99 per 355ml bottle. We are currently looking in New Mexico for a supplier of normal (gallons) of methanol. Just the same we hope we can reduce the cost of our biodiesel by recovering as much methanol as possible. We are currently buying the parts for our own Appleseed processor. We have the pump and ball valves now. Still looking for an appropriate electric hot water heater. So, my question is: How much methanol will we be able to recover from a properly functioning Appleseed processor? Is it worth the hassle?

Thanks for your time.
Brain Rodgers

i bought a new water heater from lowes a whirlpool 55 gallon tank..

i wouldnt do methanol recovery unless your a diehard biodieseler.. the energy used to recover it isnt cost effective.. plus the amount you get out isnt really great

quote:

Originally posted by Boss:
Methanol recovery?
Hi everyone.
We are now processing our third 3 liter mini batch of biodiesel. Yippee! We are becoming more familiar with the process with each batch. We ordered two kilos of KOH from Fischer Scientific, along with two lab aprons and a box of lab gloves. However, I forgot to order phenophelien as we want to go with it for titration instead of the pH meter method we began with. Now that I write this I see I have two questions. What are the different pH values that phenophelien, pheno-red and what is the other one called? Bromo- blue? Anyway, Fishersci.com seemed a bit pricey on the phenophelien. Anyone know of a good source for these? Second, with these small (3L) test batches we are using HEET and the cost is way too much, even at $.99 per 355ml bottle. We are currently looking in New Mexico for a supplier of normal (gallons) of methanol. Just the same we hope we can reduce the cost of our biodiesel by recovering as much methanol as possible. We are currently buying the parts for our own Appleseed processor. We have the pump and ball valves now. Still looking for an appropriate electric hot water heater. So, my question is: How much methanol will we be able to recover from a properly functioning Appleseed processor? Is it worth the hassle?

Thanks for your time.
Brain Rodgers

From a 30 gallon process I can recover 20-30% out of the 6 gallons of Methanol (2+ GALLON OF 99% PURE Methanol) It is cost effective as you only need heat which costs pennies per hour. You will need to make a pot still or a condensor to recover the methanol. Some people are recovering 40% of their Methanol they are using.

HTH

Ian

Don't waste your money on phenolphthalein. Click here.

And as for building a simple condenser:
http://www.liferesearchuniversal.com/condenser.html#recover

I spent about 25 bucks putting my methanol recovery system together. Used water heater, 10 ft of 1/2" soft copper tubing to make the coil, a few copper fittings, etc. The whole rig paid for itself the second time I used it. I typically do 18 gallons of byproduct and typically recover 6 gallons of meth, or a bit more. I use a lot (25%) of methanol per batch and recover the excess.

Besides, what else are you going to do with the methanol???

It's toxic and it's also a polutant. Trivial for small amounts, but you don't really want to evaporate large amounts out into the enviroment.

Finest regards,

troy

Very good replies, thank you all.
If I may take a bit more of your time, as each of you, got me thinking more in-depth.
Where does the major portion of the methanol go?
In the glycerin? Or, is whatever is not used in the chemical reaction distributed between glycerin and biodiesel? I guess what I am asking is which product is heated to evaporate the methanol? Bear in mind I am only curious at this stage.

USPS just dropped off my order from utah biodiesel, cool cool. Now I have most of the parts for my bubble washing system!

Ok I can live without phenophelien too. Turmeric huh? Ok dokkee. So we just stick with the scientific method and we'll find out when our turmeric turns from yellow to red? This brings me to another issue. What is the pH we are looking for with titration, 8.5? And is this the pH turmeric turns red or close enough?

Fed-ex just dropped off the KOH from fishersci.com Boy this company blows. They put the two aprons in one box, have not shipped the gloves and now only 500grams of the two keys KOH we ordered have arrived. It must be that I ordered it from subsidaries of fishersci. They are coming from all over the place. Oh well at least some of the stuff is getting here.

Ok last question. I promise. right?
Is it ok as far as you are aware to use copper in the methanol condenser?

I love this stuff!
Plumbing is a blast as long as I am not waste deep in crap.
Brian Rodgers

Boss

Re the methanol, the reaction consumes about 128 ml per litre of oil. Whatever you use above that is the "excess". The excess is distributed roughly 2/3 rds in the glycerine. So if you use 200ml methanol per litre of oil there will be 24ml in the fuel and 48ml in the glycerine.

Your queries about turmeric should be fully answered on the thread I linked you to above.

Thanks for the info on methanol,
Yes, I read the stuff about turmeric. I guess I needed some more reassurances. If you say it works I will give it a go. If in doubt I will try to find the phenol red. Unfortunately, there are no pool supply stores here. Plus, I saw in another area here a fine list of resources. I need to find a source for methanol here as well. I heard from a friend that a biodiesel co-op in Taos NM lost its lead movers and shakers. I will see what they are all about when I get some more info. Las Vegas NM is about fifty miles from Taos. Anyway thanks again.
Brian Rodgers

Dude,

Tumeric works and does so without fail. Just do it--it is far better than phenol red. Dirt cheap, too.

You become an advocate or your money back!

I just read this thread about distillation of the Glycerin / Meth. So is it just a matter of dumping the Glycerin into your reactor (after taping off the BD of course) and heating?
What temps must be attained?
Typically how long does it take?
What is the clean up of Glycerin residue from reactor like afterwards?
I suppose if one were to make a separate distiller that some type of vessel with a wide opening would be preferred to clean it out afterwards?
Any other tips on this procedure?
Thanks. PD

Very informative.
I have been following the links to other threads here and you are right, tons of encouragement found here and technical info too. Thanks for pointing me in the right direction(s). I will pack up the pH meter I borrowed from the local university, return it with thanks, and stop at the grocery store on the way home from work and buy a little jar of turmeric. Sweet!
This just keeps getting better & better.
Brian Rodgers

Copper is fine for your condensor coil/tube. Aluminum would be highly NOT recommended because methanol is corrosive to Al. Iron and steel would not work well because they have such poor heat transfer compared to copper. So yeah, copper's it.

Finest regards,

troy

I just got back from Lowe's where I picked up the stuff to build a condenser to recover methanol.

I bought 20 feet of 3/8" id soft copper tubing. I probably could have gotten away with 10 feet but it would have been close. This way I can have plenty of room for error.

I welded a bung to accept a water heater element into a barrel. I then took the 2" cap and welded a nipple onto it. Then I used a coupler and a brass compression fitting that, on the other end, has 3/8" npt male threads.

I'm going to try to make it so that the copper tubing stays in one piece from the compression fitting all the way out of the side of the plastic bucket a few inches to act as a spout.

If that doesn't work or I end up kinking the line or something I guess I'll just have to go get a sweat on coupler and solder it.

Back to my barrel... I was thinking about some of the treads about the time involved in heating the byproduct to the point where it starts to give up the methanol.

Has anyone installed more than one element in the barrel to speed up the heating process?

Are there any issues I should be concerned about regarding installing multiple heating elements?

Would it heat it too fast or cause more risk of fire/explosion?

My wife would never forgive me if, after her telling me not to blow up the house, I blew up the house! LOL.

Wayne

Wayne Thomas

You keep frightening me. You talk about a lot of heat input. What calculations have you done to show that the vapour stream you generate can be forced through 20 feet of 3/8 th tube without raising the pressure too much for your drum?

For high heat input you need a wide bore vapour tube. I suggest you think about using your copper tube for the cooling water.

Neutral. I'm not sure why I'm frightening you. I didn't say I was going to install 8 heater elements and fire them up tonight and I'll let you all know if I lived to see morning. I asked if anyone has done it and even asked about the risks involved with that much pressure.

I also mentioned that I bought 20 feet in case of error. That way I would sure to have enought. I didn't way I was making the thing 20 feet long. Granted it will probably be at least 15 feet long given that almost 10 feet of it will be used up just on the coil in the bucket.

How much pressure will it take to push methanol vapor through a 3/8" inside diameter piece of tubbing 20 feet long? 15 feet long? 12 feet long?

I don't have a clue as to how much pressure it is going to generate or how much a barrel will tolerate.

Enlighten me please.

Wayne

1 kg of methanol turns into about 840 litres of gas at its boiling point. This is more than anyone realizes. You want this to get through the condenser pipe with very little back pressure.

If I were making a condenser for this task I would get a couple of yards of 1.5 inch pipe and coil up your copper tube and push it inside. Preferably have a short near vertical pipe coming up out of the pot, then an elbow to the 1.5 inch pipe. Have this sloping slightly downward to your collection vessel. Run the cooling water upwards through the copper tubing. Have a thermometer at the elbow so that the bulb is just below the highest point that the vapour has to pass over. While distilling this will read the boiling point of the methanol.

You will be able to tell immediately if this condenser is adequate, or if you are heating too fast, by running your hand over the 1.5 inch pipe. It will be hot at the pot end and somewhere along its length, if adequate, it will be much cooler. the methanol delivered should be warm but not hot.

quote:

I suppose if one were to make a separate distiller that some type of vessel with a wide opening would be preferred to clean it out afterwards?

I am scheming to take a couple of 40lb propane bottles and cut the tops off such that one has a larger top cut than the other. The larger top piece becomes a bolt on top for the smaller cut tank. Obviously they must be filled with water to make this adventure safe. Once the removeable top is sealed on, the unit can then be used to vacuum distill methanol.

For those of you new to the concept ... applying a vacuum to your still (typically) lowers the boiling point of your fluids allowing you to apply less heat. You must of course maintain a temperature differential between the boiler and condenser to drive the process.

Glenn

Neutral, the only problem I have with your design is that I've already built one based on the coil in a bucket design.

What I need to know is how to figure out if my 3/8" id tubing will work.

I wanted to do the distilling this morning but I'll have to wait till I hear back from someone.

Wayne

Put a pressure gauge on the drum. Monitor it while distilling. Keep pressure under control by controlling heat input. After a couple of runs you will know what wattage it can take. Unless you have it flowing you will have to monitor the temperature of the water in the bucket too.