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Methanol Recovery IN Reacted Biodiesel with Glycerol?
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Team,

Can I do the following:
1. React biodiesel at 130 degrees F (or do an AE 2 stage reaction)
2. Once I pass my 27-3 test...
3. RAISE the temp in the reactor (with still affixed to top) to 150F or so at the head
4. Distill off the methanol from both the glycerin AND the biodiesel together by bubbling air in the bottom of the reactor (slowly). Recover the methanol through the still head via typical reflux still.
5. When finished, Remove from heat and allow the glycerol to settle and decant it off.

What should be left is biodiesel with no methanol, right?

Is this possible?
 
Registered: August 19, 2008Reply With QuoteReport This Post
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What you would be left with is demethed bio and glycerin byproduct.
This thread that Chug started may help shed a little light.http://biodiesel.infopop.cc/ev...19605551/m/989100721
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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So it seems that this would be a good move - we can therefore not waste energy waiting to decant the glycerol off and then heat it separately to remove the glycerol.

That being said, how much acid would I have to add to neutralize the acid first so I eliminate the possibility of reversing the reaction?
 
Registered: August 19, 2008Reply With QuoteReport This Post
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Originally posted by H20 Boy:
So it seems that this would be a good move - we can therefore not waste energy waiting to decant the glycerol off and then heat it separately to remove the glycerol.

That being said, how much acid would I have to add to neutralize the acid first so I eliminate the possibility of reversing the reaction?


Neutralizing the caustic that is remaining in the bio/glycerine is done by titrating the mixture with an acid solution and phenolpthalein or tumeric indicator. Add 1ml of your bio/glycerine mixture (you'll need to thoroughly mix the reactors contents before pulling the 1ml) to 10ml blanked IPA just like doing a ffa titration. Titrate the sample using an acid soultion of HCl of Sulfuric (which ever one you wish to use in neutralizing the batch). I would recommend HCl since it's not quite as concentrated. The acid solution can be made by adding 1ml of your acid (regardless of strength) to a volume of distilled water less than 1 Liter, then top off the container with distilled water to the 1 Liter mark. This makes an acid solution of 1ml acid in 1L of solution.
The sample should be purple with phenolpthalein or red with tumeric indicator added.
Titrate with the acid solution intil the color changes back to yellow with tumeric or the purple disapears with phenolpthalein. The number of ml used in the titration is the number of ml of acid you need per liter in the processor to neutralize the batch.
Adding the volume of acid in stream with the pump running over a period of time that allows the reactors contents to be circulated at least one time (preferably more) might reduce the chances of "localized soap splitting" from occuring.

Hope this helps.
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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What DD said!
See the GL push/pull thread as well as Chug's WBD method for all the nuances to this procedure.
Also note that the glycerin will settle immediately after the demething has stopped so drain the glycerin pronto, especially if you are using NAoH.
I have also noticed slightly acidic biodiesel after recovery which led me to reduce the titrated amount of acid by 50ml on a 100 litre batch. See many posts by me and others in the above mentioned threads all about it...
Good Luck!
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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Double D,

What part of Central VA are you in? I have property on the NN (Wicomico Church).

Thanks, team!

BTW, does any of this change if I am doing Acid Esterification?
 
Registered: August 19, 2008Reply With QuoteReport This Post



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BTW, does any of this change if I am doing Acid Esterification?

Nope.
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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Originally posted by H20 Boy:
Double D,

What part of Central VA are you in? I have property on the NN (Wicomico Church).

Thanks, team!

BTW, does any of this change if I am doing Acid Esterification?


I'm 30 minutes Northwest of Charlottesville.
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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double d what do you do with your waste glycerol i need to get rid of 1400 gallons can you use it on your farm
 
Location: roanoke va | Registered: December 24, 2006Reply With QuoteReport This Post
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You got a water treatment plant near by? Often they can use it in a digester to feed the microbes and it actually helps the breakdown process.



** Biodiesel Glycerine Soap - The Guide
- on 5 continents helping people make & sell soap from the Biodiesel Glycerine.


 
Location: :-) Great White North eh ? | Registered: December 10, 2004Reply With QuoteReport This Post
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Since biodiesel production is an equilibrium reaction, pulling methanol off when biodiesel and glycerol are together, a reverse reaction could theoretically occur.
 
Location: Dunnville, ON | Registered: May 01, 2012Reply With QuoteReport This Post
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The idea was to neutralise the base catalyst with acid prior to distilling off excess methanol. I don't know if its possible to exactly neutralise only the excess catalyst without producing free fatty acids from the soap that's present. No catalyst, no reaction reversal. I did it, but surely made some free fatty acids from the soap. I'm still working on whole batch demething.
 
Location: Texas | Registered: April 27, 2011Reply With QuoteReport This Post



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