Re: [biofuel] One Litre Line

2003-03-24 Thread Steve Spence

as an aside, was boiling sap this weekend for maple syrup, and came across
some really neat 15 gallon drums (half of a 30) labeled "dr. pepper", a semi
popular soft drinks in these parts. complete with bungs and everything a 30
or 55 would have.


Steve Spence
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[EMAIL PROTECTED]
- Original Message -
From: "Darryl McMahon" <[EMAIL PROTECTED]>
To: 
Sent: Sunday, March 23, 2003 10:03 PM
Subject: [biofuel] One Litre Line


> I hope some of you can help explain to me what I have seen of late.
>
> I am a biodiesel novice and no chemist.  I have spent a couple of months
now
> building my one-litre biodiesel processing "plant".  This is intended to
model my
> plans for a larger 100-150 litre setup to come later.  But I want to keep
my early
> mistakes small (and I make plenty to learn from).
>
> The reactor is a scavenged slow cooker, which does a reasonable job of
keeping the
> mixture at about 50 degrees C at the lowest setting.  Agitation is
provided by a
> discarded mix master with one beater that is lowered into the cooker while
attached
> to a plexiglas splatter shield.  The settling tank is a 1.8 litre glass
jar, and
> the washing tank is a 2-litre glass jar with 2 small air stones, a
5-gallon
> aquarium pump, plastic tubing and a large steel washer as a weight.
>
> The first batch was done with fresh vegetable oil.  I made the methoxide
using 200
> ml of methanol and 3.5 grams of lye.  The titration results were bizarre
the first
> time, and closer to the expected result the second time.  I went with Mike
Pelly's
> recommended recipe for the one-litre test batch.  I put the oil into the
reactor,
> then the methoxide.  All went as expected from my reading.  I allowed the
mixing to
> go for about an hour, then drained the lot into the settling tank.
>
> The separation began quite quickly, and after a couple of days there was a
creamy
> coloured precipitate layer at the bottom, but less than I expected.  I
estimate a
> bit less than 10% of the total volume (say about 100 ml).  Does this make
sense
> given it was fresh oil instead of waste oil?
>
> I let the batch settle for about 2 weeks, and then transferred the oil to
the
> washing tank, drawing the oil off from the top.  I noticed at this time
that there
> seemed to be some "dendritic" material, almost like wisps of white cotton
candy,
> growing up from the sediment layer.  Any ideas on what that is?
>
> Onto the washing.  I set up the washer with the stones at the bottom of
the jar,
> then added about 500 ml of tap water, more or less the Idaho method, as I
> understand it anyway.  Then I added the oil, a little over a litre, so
presumably
> containing some methanol/methoxide.  Before I started the bubbling, there
was a
> significant white layer above the water and below the oil.  Reminded me of
> mayonnaise.  I suspect a water/methoxide reaction, as I see no visible
reaction
> when I mixed methanol and water for comparison.
>
> Oh, no vinegar used.  When I was finally set to go tonight, not a drop to
be found
> in the house.  I'll be sure to correct that before the next washing.
>
> After I started the bubbling, the "mayonnaise" came to look more like
white
> aquarium stone or rock salt.  Anyway, the wash is under way now.  Bubbling
froth at
> the top was ferocious initially, but after 20 minutes it has subsided a
lot.  The
> mix is quite opaque and a dark cream colour now.  I have had to stop the
bubbling a
> little after an hour, as one of the air stones has disintegrated (12 hours
was
> recommended).  It is starting to settle out again, looks like there will
be a good
> pile of whitish precipitate once settling is done.
>
> The second batch was made from lightly used vegetable oil (to deep fry a
turkey),
> but has been stored for some time since then.  Titration indicated 1.5 ml,
so I
> used 5 grams of lye (1.5 + 3.5) and 200 ml methanol.
>
> This batch frothed some during the stirring phase, which I did not notice
with the
> first batch (fresh oil).  The separation started slower, but there is much
more
> precipitate this time (at least 25%).  However, there are a few of the
"dendritic"
> white threads suspended in the clearer oil, apparently due to having
trapped some
> bubbles which are keeping them buoyant.  I'm sure they'll filter out in
the next
> transfer.
>
> So, now that I actually have some experiences to report, I would also like
to thank
> Tom Leue for putting up with us for an afternoon last November when we
brought the
> snow to Massachusetts.  His tour of the facility and advice were, and are,
much
> appreciated.
>

[biofuel] One Litre Line

2003-03-23 Thread Darryl McMahon

I hope some of you can help explain to me what I have seen of late.

I am a biodiesel novice and no chemist.  I have spent a couple of months now 
building my one-litre biodiesel processing "plant".  This is intended to model 
my 
plans for a larger 100-150 litre setup to come later.  But I want to keep my 
early 
mistakes small (and I make plenty to learn from).

The reactor is a scavenged slow cooker, which does a reasonable job of keeping 
the 
mixture at about 50 degrees C at the lowest setting.  Agitation is provided by 
a 
discarded mix master with one beater that is lowered into the cooker while 
attached 
to a plexiglas splatter shield.  The settling tank is a 1.8 litre glass jar, 
and 
the washing tank is a 2-litre glass jar with 2 small air stones, a 5-gallon 
aquarium pump, plastic tubing and a large steel washer as a weight.

The first batch was done with fresh vegetable oil.  I made the methoxide using 
200 
ml of methanol and 3.5 grams of lye.  The titration results were bizarre the 
first 
time, and closer to the expected result the second time.  I went with Mike 
Pelly's 
recommended recipe for the one-litre test batch.  I put the oil into the 
reactor, 
then the methoxide.  All went as expected from my reading.  I allowed the 
mixing to 
go for about an hour, then drained the lot into the settling tank.

The separation began quite quickly, and after a couple of days there was a 
creamy 
coloured precipitate layer at the bottom, but less than I expected.  I estimate 
a 
bit less than 10% of the total volume (say about 100 ml).  Does this make sense 
given it was fresh oil instead of waste oil?

I let the batch settle for about 2 weeks, and then transferred the oil to the 
washing tank, drawing the oil off from the top.  I noticed at this time that 
there 
seemed to be some "dendritic" material, almost like wisps of white cotton 
candy, 
growing up from the sediment layer.  Any ideas on what that is?

Onto the washing.  I set up the washer with the stones at the bottom of the 
jar, 
then added about 500 ml of tap water, more or less the Idaho method, as I 
understand it anyway.  Then I added the oil, a little over a litre, so 
presumably 
containing some methanol/methoxide.  Before I started the bubbling, there was a 
significant white layer above the water and below the oil.  Reminded me of 
mayonnaise.  I suspect a water/methoxide reaction, as I see no visible reaction 
when I mixed methanol and water for comparison.

Oh, no vinegar used.  When I was finally set to go tonight, not a drop to be 
found 
in the house.  I'll be sure to correct that before the next washing.

After I started the bubbling, the "mayonnaise" came to look more like white 
aquarium stone or rock salt.  Anyway, the wash is under way now.  Bubbling 
froth at 
the top was ferocious initially, but after 20 minutes it has subsided a lot.  
The 
mix is quite opaque and a dark cream colour now.  I have had to stop the 
bubbling a 
little after an hour, as one of the air stones has disintegrated (12 hours was 
recommended).  It is starting to settle out again, looks like there will be a 
good 
pile of whitish precipitate once settling is done.

The second batch was made from lightly used vegetable oil (to deep fry a 
turkey), 
but has been stored for some time since then.  Titration indicated 1.5 ml, so I 
used 5 grams of lye (1.5 + 3.5) and 200 ml methanol.

This batch frothed some during the stirring phase, which I did not notice with 
the 
first batch (fresh oil).  The separation started slower, but there is much more 
precipitate this time (at least 25%).  However, there are a few of the 
"dendritic" 
white threads suspended in the clearer oil, apparently due to having trapped 
some 
bubbles which are keeping them buoyant.  I'm sure they'll filter out in the 
next 
transfer.

So, now that I actually have some experiences to report, I would also like to 
thank 
Tom Leue for putting up with us for an afternoon last November when we brought 
the 
snow to Massachusetts.  His tour of the facility and advice were, and are, much 
appreciated.

So anything you can tell me about what I have described, or any mistakes you 
can 
see I am making, please let me know.

Darryl McMahon






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