[biofuel] Re: Two-stage Process - jelly?

2003-05-29 Thread girl_mark_fire

mark,
I;'m not surprised that you don't have a 'glycerine' layer after the 
first stage.
First of all, the more I think about it,  the more I doubt that it's 
glycerine you sometimes see in the bottom of the container at 
the end of the first stage- someone correct me again if I'mn 
wrong- but if it's an esterification of free fatty acids, rather than a 
transesterification of an intact triglyceride, it seems to me that 
there wouldn't be much glycerine breaking off other than the very 
small amount of trans-e that's (very slowly) occurring.  

Jon Van Gerpen's research on this process considers this layer 
to be excess methanol, combined with some water that is 
formed in the reaction. Presumably there'd also be a little bit of 
glycerine if any transesterification is happening as well, all in the 
same layer as the water/methanol.

I believe that Todd also calls it first stage methanol rather than 
first stage glycerine, and if you look at how 'runny' it is, it looks 
like methanol more than like glycerine (at least the few times Ive 
seen it). 

Van Gerpen's method (that's the exceedingly-high-methanol 
industrial process, somewhat different than Aleks' process and 
hard to do if you don't have methanol recovery and cheap energy) 
finds that depending on the amounts of methanol used and the 
amounts of water produced, the excess methanol/.water 
sometimes coalesces on top of the esters/oil, and sometimes 
ends up below the oil phase. The stuff I saw/made using his 
method created a layer that looked exactly like the watery 
'glycerine' that I've seen using A;leks' method. However I have not 
always produced this aqueous layer in Aleks;' method, and I 
frequently used that method with nice oil, just like you. So my 
guess is that it's somehow connected to the amount of water 
produced, and that the condition of the nice oil might have 
something to do with it. I would also guess that  how dry the oil is 
in the first place would be a contributing factor.
Anyway, I don't worry when I don't see first stage glycerine in 
ALeks method, as that seems quite normal to me in my 
experience. On the other hand I usually don't look for it, so it may 
appear more often than I am aware of.

Todd in the post below suggests removing any first stage 
alcohol (the dark layer, sometimes below and sometimes above 
the oils).I would add that if you do this change, be prepared to 
add a similar amount of fresh, anhydrous methanol, to replace 
any that is removed, to make sure there is enough for the 
second stage reaction. 

mark

--- In biofuel@yahoogroups.com, Appal Energy 
[EMAIL PROTECTED] wrote:
 Mark,
 
 Earlier I was curious if you were using oil or an oil/fat blend 
(WVO).
 Should it be presumed that the feedstock at the beginning of 
the second
 stage and prior to reheating is still liquid? If so, should it be 
presumed
 that there was a layer of extra alcohol above the oil, perhaps 
slightly
 darkened?
 
 If so, and were it me, I'd separate the feedstock from such a 
layer and then
 conduct the second stage, just to isolate variables. Second, if 
you're
 getting jelly out of a SVO, you might wish to back off the 
caustic some.
 Jelly, or glop soap is a condition that results from too much 
caustic in the
 presence of water. It doesn't take much to push what is 
primarily a
 transesterification reaction into one that is directed towards
 saponification (soap making, aka jelly).
 
 You might (or perhaps might not) care to take a look here.
 http://groups.yahoo.com/group/Biodiesel/message/2504  It's a 
step by step
 how to that runs the base side of an acid base experiment in 
three
 separate stages, rather than all at once.
 
 That's not to declare that it should be done in such a manner. 
But it does
 indicate that glycerin drop in the second stage can occur with 
less than a
 requisite amount of caustic.
 
 Take your time and take no short cuts. It works and works well.
 
 Todd Swearingen
 


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[biofuel] Re: Two-stage Process - jelly?

2003-05-28 Thread girl_mark_fire

Check that you are not accidentally evaporating off too much of your 
methanol. What kind of container are you using on that hot plate? If 
it is an Ehrlenmeyer flask you've got a better chance of retaining all 
the methanol than if you are using a beaker, for instance. If you put 
a lid over the container you're better off still.

mark


--- In biofuel@yahoogroups.com, mark schofield [EMAIL PROTECTED] 
wrote:
 Hi
 
 So after playing with the single stage for a
 while, I have produced a good clear final
 product. I have bought a hot plate magnetic
 stirrer for $360 USD that has helped for
 titrations etc


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Re: [biofuel] Re: Two-stage Process - jelly?

2003-05-28 Thread gobie


- Original Message -
From: girl_mark_fire [EMAIL PROTECTED]

 Check that you are not accidentally evaporating off too much of your
 methanol. What kind of container are you using on that hot plate? If
 it is an Ehrlenmeyer flask you've got a better chance of retaining all
 the methanol than if you are using a beaker, for instance. If you put
 a lid over the container you're better off still.

 mark

A glass funnel placed in the neck of the Ehrlenmeyer flask acts as a nice
condensor. If you want to get fance the neck of the funnel can be blocked at
its tip and the funnel filled with crushed ice, but that should not be
necessary..

Regards,   Paul Gobert.



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