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Put 500 ml new corn oil in a flask. Added 200 ml dry methanol and 4.2 ml concentrated sulfuric acid. Heated about 11 hours at 60-63 degrees centigrade with magnetic stirring. To get a two layer (phase) liquid product. Added 17.7 grams 85% KOH dissolved in 125 ml dry methanol with magnetic stirring. Heated about four hours at 59-60 degrees centigrade with magnetic stirring. Set the 1 litre round bottom stoppered flask in a dark closet at 70 degrees farenheit for three days. Then four phases (layers) formed, an upper alcohol layer approximately 200 ml, a middle biodiesel layer, a lower glycerine/ water layer and a lowest potassium sulfate solid crystal layer. Four phases (layers). I didn't expect this. Its pretty cool.
 
Location: Texas | Registered: April 27, 2011Reply With QuoteReport This Post
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I removed the lower solid crystal layer and the glycerine layer leaving the two upper layers (phases). I vacuum distilled out about 126 ml of methanol from the upper two layers to get a still bottom that formed two layers. The still bottom was 525 millilitres. Poured the still bottom into a separatory funnel where after sitting it formed two phases. 100 ml of the lower phase weighed 92.9 grams. 100 ml of the upper phase weighed 87.35 grams. I measured out about 240 millilitres of upper phase crude product. Based on the density the upper phase is crude biodiesel and the lower phase is soap, unreacted corn oil, and other stuff. The upper phase was transparent when it was in the separatory funnel but became translucent when I poured it into a 100 milliliter graduated cylinder. I previously measured the density of new corn oil at 0.915 grams per millilitre. On the internet I found that the density of biodiesel is about 0.87-0.88 grams per millilitre. A conclusion I reach is that in Acid Esterification followed by base transesterification water is produced upon the neutralization reaction that can hinder the base transesterification reaction by decomposing methoxide and reducing the presence of methoxide due to the increased content of water. From new corn oil I got 48% by volume of crude biodiesel product. I wonder how the AE people get around the water produced by neutralization killing the base transesterification reaction. Thanks. I took my 240 ml of crude biodiesel, water washed then dried with anhydrous sodium sulphate. Then further purified with 10 grams magnesium silicate to get 180 millilitres of purified methyl biodiesel with a measured density of 0.877 grams per millilitre. I've wondered what the density of biodiesel from corn oil should be, so I took extra trouble to purify it before measuring the density of my product.

This message has been edited. Last edited by: WesleyB,
 
Location: Texas | Registered: April 27, 2011Reply With QuoteReport This Post
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hello westley,
I always enjoy reading your posts. I have been converting corn oil now for a few mounths and using a.e. I would like to let you know a little info on how i have been doing this. usual initial oil is about 5000 ppm moisture and starts with an ffa of 13 to 14. I first vacuum distill the moisture until under 4000 ppm or less. and then find the mass of ffa, by taking the ffa and turning it into a decimal. ( 12.5 ffa = .125) then times that by the batch size in lbs. that is the mass of the ffa. I then times the Mass of ffa with a multiplier of about 1.1 for the dry methanol in lbs. divide this by 6.58 to get gallons. I use inbetween 2-5% of h2so4 against the mass of ffa. after a reaction of 4 to 5 hours at 62 - 65 c I neutralize the acid. then vacuum distill until under 1000 ppm moisture. then go into trans. try this and you should not have so much soap and water!

Cooper
 
Location: Bioville Ohio | Registered: June 30, 2010Reply With QuoteReport This Post
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for ae to work affectively you need to get the water content of the oil down to 500ppm or less!


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Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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