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Kurt,
You wrote:
" ... Emulsed like crap when I tried to wash it, to the point
of a full 50% of the test wash ending up a crappy mayonnaise consistency.
To date, after 36+ hours of settling, I barely have 100mL of clear upper level
separated out of a 300mL test wash."
........
(my underline)
The "crappy mayonnaise"
sounds like soap.
"Added a very carefully measured amount of my
methoxide, 100mL, to the reprocessing candidate in the blender."
.......
"Anyway, five hours after reprocessing the first-run
product, ... "
Did any additional
glycerine fall out? ... Would suggest an incomplete reaction. If not, it would
further suggest soap.
"I drew out another 100mL and added 100mL of hot
(120~F) water. Gently swirled it at first, but that wasn't even mixing water and
product so I went to a slightly more vigorous shaking. And it did the same
thing. Emulsed like crap. I have a 200mL jar of two-tone mayonnaise. The upper
layer is tinged yellow-brown, the bottom layer is pure white."
As I understand it, emulsions are
caused by soap due to water in the reaction or failure to separate glycerine out
prior to wash, or by unreacted glycerides due to an incomplete
reaction.
It sounds like you got
soap ... a lot of it.
I don't think reprocessing
will help if you made soap in the initial reaction.
Minimize soap by keeping
water out of the reaction. Make sure the oil is dry. (See JtF: "Removing
Water"). Use good methanol and lye. Give adequate time for glycerine mix to
settle and err on the side of "losing" BD when you separate the
two rather than risk glycerine in the BD that you want to wash. (Recover BD
later). Measure lye accurately. Being off by .5 to 1.0 g on a 1L batch is more
significant than being off the same amount on a 50L batch.
Being new to BD
production, I claim no expertiese, but the heartbreak of emulsions is still
fresh in my mind. My first large (30 gal) batch ----> large emulsion.
Following suggestions, I salvaged the batch, tweated the process and have been
making 20 gal batches that wash easily (stir-wash) and when a small sample is
reprocessed -----> little if any additional glycerine.
It is possible to make
high quality BD following the instructions at JtF.
Solving problems that
arise is part of the process.
In your case it may simply involve a better balance
for measuring lye. Check out how to break emulsions at JtF.
Best Wishes,
Tom
Sent: Monday, October 10, 2005 12:28
AM
Subject: [Biofuel] Alright, I'm
stumped.
Okay, so earlier this week I tried my first batch. Didn't go so
hot, it was still a little cloudy after I was done. Emulsed like crap when I
tried to wash it, to the point of a full 50% of the test wash ending up a
crappy mayonnaise consistency. To date, after 36+ hours of settling, I barely
have 100mL of clear upper level separated out of a 300mL test
wash.
Okay, so I figured I screwed up along the line somewhere. I had
some doubts as to the unused status of the oil, so I looked up the directions
and reprocessed a liter of it in a blender.
I mixed up a large enough
batch of the 10% methanol blend suggested for reprocessing for my little scale
to be accurate (It only measures in 2g increments. Must find a better scale!)
and I did it inside where the humidity was only around 60% (As opposed to
exterior humidity of around 90%+) and quickly, only taking a bare 45sec to a
minute from the time I opened the cannister to the time NaOH hit the methanol
in the blender bowl. It mixed rather nicely, and I pulsed it's mixing off and
on to keep the blender cool during the fifteen minutes it took me to be
confident everything had fully dissolved. It ended up a very
<i>slightly</i> cloudy mixture, but nothing settled into the
bottom over the next hour.
During the course of that hour I set up the
other stuff, measuring out a liter of my initial product, putting it in a
second blender (Just bought it, cheap $14 one), getting that all set up; it
was still slightly cloudy when I put it in the blender. During this same time
I also measured out 500mL of just-purchased canola oil, intending to process a
real minibatch after I reprocessed some of my initial product.
Added a
very carefully measured amount of my methoxide, 100mL, to the reprocessing
candidate in the blender. Snapped the lid on, made sure everything was secure,
and let her go. Twenty minutes of blenderized thrashing commenced, during
which time the whole slew became a kind of milky yellow-amber color, with a
brown tint to it. Cut the blender off, poured everything inside it out into a
glass jar with a cap.
Set that aside and went into the house, washed
the blender cup thoroughly, inside and out. I towelled it off, then let it
air-dry for a good five or ten minutes inside the house. Took it back outside,
put it back together, and added my fresh oil to the cup. Drew out another 50mL
of my 10% grade solution, adding another 50mL of my methanol source to bring
it up to the requisite 20% volume. Since the grams of lye per liter were never
changed, just the volume of methanol, I reasoned that doing this was safe and
would work since I was just bringing the lye concentration down to normal by
diluting the solution with more methanol.
Added this to the batch of
fresh oil, secured the cap, turned the blender on and walked inside to wash my
hands again and get something to drink. Ten minutes later I walked back out,
and the blender was utterly empty. Bottom end failure on my cheap blender;
apparently I hadn't let the motor cool long enough, so the heat ran up the
shaft and when combined with the heat of mixing it I melted the plastic.
Bummer. So I don't have that as a comparison.
Anyway, five hours after
reprocessing the first-run product, I drew out another 100mL and added 100mL
of hot (120~F) water. Gently swirled it at first, but that wasn't even mixing
water and product so I went to a slightly more vigorous shaking.
And it
did the same thing. Emulsed like crap. I have a 200mL jar of two-tone
mayonnaise. The upper layer is tinged yellow-brown, the bottom layer is pure
white.
Ummm, help?
-K
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