Problem seeing bio/glycerine layer
#1
Problem seeing bio/glycerine layer
After some research and encouragement, I changed from NaOH to KOH. All I have made so far are lab scale batches until I get the process down. I have calculated the difference for the KOH (X1.4%), done the titration with the KOH/distilled water, blended this with the 99% methanol and done the reaction. The result was unnoticeable at first. The "bio" layer and the glycerine layer are so close in color that they are almost indistinguishable. I have tried varying levels of KOH. The most straw colored bio I received was about a 20% conversion before the product turned dark. I have tried the same WVO with the red devil lye and received the same result. In the past, I had great success with the NaOH, but the oil was not used nearly as much. My supplier is a MDs in the area and the titration yielded 9.5g/L!!! Is there an intermediate step possible to neutralize the FFA's before attempting the conversion, so I may be able to distinguish between product and byproduct?
Thank you in advance,
Ben
Thank you in advance,
Ben
#2
[QUOTE=wbw189]After some research and encouragement, I changed from NaOH to KOH. All I have made so far are lab scale batches until I get the process down. I have calculated the difference for the KOH (X1.4%), done the titration with the KOH/distilled water, blended this with the 99% methanol and done the reaction. The result was unnoticeable at first. The "bio" layer and the glycerine layer are so close in color that they are almost indistinguishable. I have tried varying levels of KOH. The most straw colored bio I received was about a 20% conversion before the product turned dark. I have tried the same WVO with the red devil lye and received the same result. In the past, I had great success with the NaOH, but the oil was not used nearly as much. My supplier is a MDs in the area and the titration yielded 9.5g/L!!! Is there an intermediate step possible to neutralize the FFA's before attempting the conversion, so I may be able to distinguish between product and byproduct?
Thank you in advance,
There is a 2 step acid/base process to reduce FFA's but is difficult for home brew. Journey to Forever website discribes it, but it has been discredited. I had a similar problem when I first started. I found if I blend my high titration oils with my low titration oils it takes less KOH to make a complete reaction.
Since switching to KOH I'm using 13.44 grams/ liter, 3lbs-1344 grams per 100 liters/25gal oil. At a mix temp of 150 deg F mixed for 30 min it will start to seperate in 10-15 min.
FABMANDELUX.
Thank you in advance,
There is a 2 step acid/base process to reduce FFA's but is difficult for home brew. Journey to Forever website discribes it, but it has been discredited. I had a similar problem when I first started. I found if I blend my high titration oils with my low titration oils it takes less KOH to make a complete reaction.
Since switching to KOH I'm using 13.44 grams/ liter, 3lbs-1344 grams per 100 liters/25gal oil. At a mix temp of 150 deg F mixed for 30 min it will start to seperate in 10-15 min.
FABMANDELUX.
#3
Thanks, Fabman. I have been marginally successful in my "lab" with an appropriate amount of conversion (75%). My stir plate was set to 500 RPM and 55C. A cream colored product agitated in a sample container for just over 5 minutes and just as quick as you could snap your fingers, the product went dark brown. Is this similar to what you have seen?
I sure do appreciate your information.
Ben
I sure do appreciate your information.
Ben
#4
Originally Posted by wbw189
Thanks, Fabman. I have been marginally successful in my "lab" with an appropriate amount of conversion (75%). My stir plate was set to 500 RPM and 55C. A cream colored product agitated in a sample container for just over 5 minutes and just as quick as you could snap your fingers, the product went dark brown. Is this similar to what you have seen?
I sure do appreciate your information.
Ben
I sure do appreciate your information.
Ben
FABMANDELUX.
#5
Yes, that is the same reaction happening, but my final product is not pale yellow. The product looks more like a dark ale. The only way I can tell the difference is to have a light source behind the flask I mixed it in and the bio is transparent. This made me wonder if I used the wrong amount of lye or if I missed a step.
Ben
Ben
#6
Originally Posted by wbw189
Yes, that is the same reaction happening, but my final product is not pale yellow. The product looks more like a dark ale. The only way I can tell the difference is to have a light source behind the flask I mixed it in and the bio is transparent. This made me wonder if I used the wrong amount of lye or if I missed a step.
Ben
Ben
If your trying small batches, try adding 50 percent more Lye. If you get a good reaction you can adjust down from there.
The only other thing it could be is over-used oil. If the WVO is light colored than the bio will be light. If it is very dark the bio will be dark.
FABMANDELUX.