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gilfish
Member
Posted
just made my first dud batch, usual animal fat filtered to approx 100 micron heated to 122f & no water present. Titrated to 9.5 koh 83 litres oil 9.5-3=6.5 x 0.2= 1.3ml/l oil = 105ml h2so4 in 10L methanol. Introduced at 50c over 45min, normally it would reach 2.0-3.5 in around 5-8hrs. Titrated after two hrs and it had gone up to 11.5 this was 13 hrs ago and it is still at 11-12 titration i think it has reversed the reaction backsplitting i think dunno. So my questioin what to do in the morning if it is still high tit. do i add more meth say a litre or more h2so4 25 ml maybe or just go to base
The only difference between this batch and the others was i had put approx 2-4 litres of glycerol/biodiesel/meth in one of the drums of fat. Which changed its viscosity from solid to semi solid thick cream consistency and the starting temps of 122 is 10 degrees above my normal start temp it pushed the process temp to 134f what to do ?
 
Location: south australia | Registered: 17 November 2008Reply With QuoteEdit or Delete MessageReport This Post
dkenny
Member
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I would suggest putting in more methanol. maybe about 2 Liters.

-dkenny


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Location: RTP, North Carolina | Registered: 15 December 2004Reply With QuoteEdit or Delete MessageReport This Post
gilfish
Member
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thanks dkenny i took a chance and put in 1.5l but nothing happened i believe one of the drums of fat /lard had water in it. So next i put 80ml h2so4 in 2l methanol and tried a again but this did not work so now i have decided to go to base/base and suffer a lot of soap/glyc have just tried 1000grams in 5l methanol but still no seperation so will put in the remainder 700grams of koh in 5l methanol after removing 5l from the bottom and hope for something this is my first failure from 13 batches of acid/base using your method/recipe so i am indebted to you,it failed due to my lack of diligence but a good learning curve thank you again andy
 
Location: south australia | Registered: 17 November 2008Reply With QuoteEdit or Delete MessageReport This Post
Green energy
Member
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Just start to study the acid reaction method. Readed a lot of post and find this one.

I guess the problem is you put 2-4 liters of glycerol in the fat. We know that there is a lot of KOH/NaOH in the glycerol if you didn't neutralize the extra KOH/NaOH after the biodiesel production.

The KOH in the glycerol will neutralize the H2SO4 which you using as catalyst. That's why the titration still keep high although you heat for a long time. Because no Acid as catalyst actually.

Any comments?


quote:
Originally posted by gilfish:
just made my first dud batch, usual animal fat filtered to approx 100 micron heated to 122f & no water present. Titrated to 9.5 koh 83 litres oil 9.5-3=6.5 x 0.2= 1.3ml/l oil = 105ml h2so4 in 10L methanol. Introduced at 50c over 45min, normally it would reach 2.0-3.5 in around 5-8hrs. Titrated after two hrs and it had gone up to 11.5 this was 13 hrs ago and it is still at 11-12 titration i think it has reversed the reaction backsplitting i think dunno. So my questioin what to do in the morning if it is still high tit. do i add more meth say a litre or more h2so4 25 ml maybe or just go to base
The only difference between this batch and the others was i had put approx 2-4 litres of glycerol/biodiesel/meth in one of the drums of fat. Which changed its viscosity from solid to semi solid thick cream consistency and the starting temps of 122 is 10 degrees above my normal start temp it pushed the process temp to 134f what to do ?
 
Registered: 17 February 2009Reply With QuoteEdit or Delete MessageReport This Post
Green energy
Member
Posted Hide Post
I guess I was wrong. Because if there is KOH/NaOH in the glycery, then before you put the H2SO4, the KOH/NaOH will react with the FFT to form soap and the titration will decrease. Then you put H2SO4, the titration will decrease further.

So I guess maybe there is some water in the by produt(glyncerol+water+...), the water will resist the FFA transfer to biodiesel

R-C(OOH)+CH3(OH)<->R-C(OOCH3)+H2O

Since the reaction can go both way, more water will resist the FFT transfer to biodiesel.

Just a guess. Any comments is wellcome.


quote:
Originally posted by Green energy:
Just start to study the acid reaction method. Readed a lot of post and find this one.

I guess the problem is you put 2-4 liters of glycerol in the fat. We know that there is a lot of KOH/NaOH in the glycerol if you didn't neutralize the extra KOH/NaOH after the biodiesel production.

The KOH in the glycerol will neutralize the H2SO4 which you using as catalyst. That's why the titration still keep high although you heat for a long time. Because no Acid as catalyst actually.

Any comments?


quote:
Originally posted by gilfish:
just made my first dud batch, usual animal fat filtered to approx 100 micron heated to 122f & no water present. Titrated to 9.5 koh 83 litres oil 9.5-3=6.5 x 0.2= 1.3ml/l oil = 105ml h2so4 in 10L methanol. Introduced at 50c over 45min, normally it would reach 2.0-3.5 in around 5-8hrs. Titrated after two hrs and it had gone up to 11.5 this was 13 hrs ago and it is still at 11-12 titration i think it has reversed the reaction backsplitting i think dunno. So my questioin what to do in the morning if it is still high tit. do i add more meth say a litre or more h2so4 25 ml maybe or just go to base
The only difference between this batch and the others was i had put approx 2-4 litres of glycerol/biodiesel/meth in one of the drums of fat. Which changed its viscosity from solid to semi solid thick cream consistency and the starting temps of 122 is 10 degrees above my normal start temp it pushed the process temp to 134f what to do ?
 
Registered: 17 February 2009Reply With QuoteEdit or Delete MessageReport This Post
marvingvx
Member
Posted Hide Post
Try letting it settle and drain the mud off the bottom possibly more than the volume of glycerol you first put in. You will know when the drain off smell doesn't curl your nose hair's.
 
Registered: 30 August 2008Reply With QuoteEdit or Delete MessageReport This Post
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