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Help me please .... my story is a long
one.
My
1st attempt at making biodiesel was a 2 L. test batch using virgin corn
oil. Shake test came out OK; bubble washed - produced clear golden
biodiesel.
Repeat
using 2L fryer oil ----> honey amber biodiesel.
I then did two
separate 15 L batches in a closed container, using pump agitation at 125 F for
40 minutes. There was a clear separation of "biodiesel" and glycerine cocktail
within minutes, I let it settle overnight. I put equal amounts of
"biodiesel" and water in a bottle and shook it up. Got clear separation within
15 minutes - this I took to be a good sign There was only a very thin film
(soap?) between the biodiesel and the water, so I proceeded to wash the
biodiesel.
I used the same pump and
hoses after flushing them out with hot water to remove any glycerine residue.
Since I didn't have any large containers at the time, I kept the two batches
separate .... doing separate washes. I pump-washed using 5 L of well water that
had been warmed to about 80 F. All seemed to go
well ... the water and biodiesel began to separate within minutes. I let it
settle for 3 hours and then drained off the water. After three washes with
fresh, clear water, the wash water was still milky. Growing impatient, I washed
one of the batches with equal volume of water and biodiesel and got an
emulsion. I broke the emulsion using vinegar. I heated the biodiesel to about
125 F and additional water "fell out". I drained off the water
allowing some of the biodiesel to come through. The water and biodiesel were
both clear and there was no soap whatsoever. I performed a shake test on
the biodiesel ---> water clear, no soap.
While this was going
on I had washed the second batch using 5 L. of warmed well water as I
had done for the first 3 washed.... no emulsion, but the wash water still
was milky.
After recovering the
biodiesel from the emulsion I washed it (5th time) using 5 L. of clean,
warmed well water ----> no emulsion, but still milky wash water.
Finally a question: The emulsion ... Is this why
directions call for 1/4 - 1/2 volume of water to Biodiesel during
each wash? (Larger volumes of water cause problems?)
Tired of washing two
separate batches, I visited my town's scrap metal pile and got a water
heater that I rigged up as a wash tank. I combined the two batches and during
the past two days I have washed the biodiesel 3 more times using 12 L of warmed,
clean well water and letting the water settle for 10 or more hours each time.
This morning ... still milky.
Each time I drain
the wash water a small amount of biodiesel comes out. I recovered the biosiesel
and after heating it to remove water, It is crystal clear and honey colored.
I have attempted to
determine pH of the biodiesel as follows: Dissolved biodiesel in isopropanol,
add water, shake vigorously. Wide range pH paper changed color .. to pH of
7.
Of course, I did add vinegar to one of the batches
and this probably neutralized impurities..... the wash water is still milky -
not murky or cloudy.
I am at a point
where I'm not sure that I am thinking clearly and could use advise.
Are the problems in the
wash telling me that my production was faulty or is there something wrong with
the wash itself?
Note: My titatration came
out to be just 2.1 g lye/liter of oil. I thought that was low, so I repeated it
twice more using fresh, 99% pure NaOH (1 g/L distilled water).
(2.1g/L +
3.5g/L ) X 15L/batch
I used 3L of fresh
methanol/15L batch (from a drum of methanol that was opened only the day
before).
Temp during reaction was
monitored by a automobile temp gauge.
What am I doing
wrong?
What do I do now? Will the wash
water ever come out clear?
I apologize for the
long-winded account. If you have gotten this far I thank you and admire your
patience and endurance.
Thoughts are
appreciated
Tom
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