A while back I tried to shake up the methoxide and oil in a closed container (due to lack of glass blender or lab stirrer), and much like a shaken soda bottle it expanded a bit and "fizzed " out a bit. I am looking for a better test setup that can prevent this type of thing. Would stirring the mixture rather than shaking it prevent this?

On 2/16/06, Charles List <[EMAIL PROTECTED] > wrote:
Yup

He's basically refluxing it, I assume, with the liebig condenser vertically attached to the reaction vessel. A closed container would do the same thing!

A good use for the liebig condenser would be to reclaim the excess methanol from the glycerine, but they are usually pretty small, so would take a while.

Charles List


On 17/02/2006, at 7:27 AM, Jared (RogueOP Productions) wrote:

How did you utilize the liebig condensor? Wouldnt that condense the gas given off by the reaction into a liquid? Is that the jist of it? Turning it into a less volitile liquid instead of a gas?

On 2/15/06, Duarte Nuno Januário < [EMAIL PROTECTED]> wrote:
Hi all!

 

 

I've been trying (made 5 batches) to produce biodiesel in a laboratory, for educational purposes. This is what I've been doing:

 

-         1 liter of virgin oil from supermarket
-         200 mL of methanol
-         3,5 grams of sodium hydroxide
-         Prepared the sodium metoxide by stirring for 24 hours (magnetic stirrer) in an closed Erlenmeyer
-         Preheated the oil to 55ºC
-         Using a flask with an attached Liebig condenser (to prevent methanol vapors to escape), mixed vigorously for 1 hour maintaining agitation and constant temperature (eventually drops to 52ºC when the metoxide is added) and maybe rising to a maximum of 60ºC at some instants.
I do get a clear phase separation after 24 hours, but my biodiesel isn't crystal clear.
When I mix a sample of the unwashed biodiesel with water and shake it, the emulsion won't separate…. It will after some hours, but with a lot of soap formation, widespread in the container.
I'm using good reactants (not p.a. but trustworthy) and anhydrous conditions.

 

There one thing I should say: I never got all the sodium hydroxide to completely dissolve in the methanol. No matter how long I keep stirring, it simply won't dissolve quantitatively. But I do filtrate the remains of solid hydroxide. Do you think this can be the problem? How can I solve it?

 

What can I be doing wrong? Why do I keep getting all this soap? Where do you think the problem might be? In a reactant? Bad quality oil? Do you think I should titrate the virgin oil?

 

Thank you all for your attention

 

 

Duarte Nuno

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