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Its not working ! Help please
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Guys,

I use Phenol red to titrate with.

My oil which is from the same supplier always titrates at 8.

I have used the new DKenny method - 250 litres of oil

Starting titration =8
desired endpoint = 2

using a multiplier of .18 - i therefore need

.18 x 250 x (8-2) = 270ml of Sulphuric (98% pure)

I added this to 30 litres of Methanol and introduced to the oil at 50c

I left this to mix overnight (12+ hours)

The titration still seems to be at 8

Rather than mess around anymore can i just move to adding the remaining Methanol and the KOH to process as normal and then come back later to work out why the process is not working. ?

I have dried my oil prior to starting - heated to 80c and sprayed through a brass nozzle for 6 hours until no more vapour was released. Passed the HPT after this with no issues.


regards

Craig
 
Registered: May 30, 2007Reply With QuoteReport This Post
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if you wish, you can proceed to base but the yeild will realy suck. the formula you used does not take into concideration that each processor contains residual caustic which can kill the ae. do yourself a favour on the next batch, use 3 ml of acid/ltr of dry oil, after adding the methanol/acid mix for 1/2 hr, 1 hr max then let sit overnight. In the morning drain 2 ltrs from the bottom before you mix, if creamy to buterscotch colour your oil was wet, drainage should be very dark to black, then mix well and titrate. Once you have mastered ae with this amount of acid start reducing the acid amount by 1/2 ml / ltr of oil until you find the minimum amount of acid that will work in your set up. Hop this hepls.


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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thanks BIOTOM.

I do not think the issue is residual caustic - my processor is an open top design - when i load the oil in i give it a water wash and dry in the processor - this should (hopefully) clean out the processor before i do the titration.

I still have the batch in the processor - it has slightly seperated but nowhere near finalised. I will dry and add more caustic and methanol tomorrow.

usually from 250 litres oil i get 175 litres of BIO so will use that as the basis for my next one with acid.

Craig
 
Registered: May 30, 2007Reply With QuoteReport This Post
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There may have been suspended moisture in your oil.
Don't mix for the whole time. As Tom said, mix then let sit.
Keep the mixture as warm as possible throughout the reaction period.
Drain a litre or two of gloop from the bottom of the reactor before remixing then test the new titration.
 
Location: Sydney | Registered: May 23, 2005Reply With QuoteReport This Post
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one of three things, caustic wet oil, lack of heat, or a combination of these. there are no other impediments to ae that I am aware of. looking at your process of washing higher ffa oil I'm thinking WET oil. diglycerides or mono glycerides, which can be abundent in higher ffa oils, attract and hold water. Tom

This message has been edited. Last edited by: Biotom,


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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This is summer as well. How is the humidity where you are Craig?
 
Registered: February 25, 2010Reply With QuoteReport This Post



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Guys,

Winter where i am - Sydney - into spring now and about to do another sample batch of 100 litres.

Lost confidence along the way - but have gone back to basics and had another good 1/2 dozen batches - so my next one is going to be AE again.

To summarize

1) Wash reactor to get rid of any residual caustic
2) Add oil
3) heat and dry
4) Titrate
5) add 300mls acid (98%) to 100 litres of oil at 45 degrees celsius
6) Add 12 litres of methanol
7) Mix for 1 hour and then let sit overnight - keep temp up past 38c all night
8) drain bottom 1 litre
9) mix for 10 minutes and then titrate

Does this sound OK ?

Craig
 
Registered: May 30, 2007Reply With QuoteReport This Post
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well no..

in the first post you used 250l of oil..the last 100l of oil..
if the titration is the same the amount acid should be lower..300mls is a LOT OF ACID..for 100l of oil or 3ml/liter..

if your using 100l of T8(KOH) oil..5*0.18 = 0.9 or 90 mls of acid not 300mls...for 250l of oil its 225..not 300 and not 250..IF IN DOUBT USE LESS ACID...you cannot remove the acid once added..unless the mix settles to the bottom, then you can drain some out..

if you're going to wash the reactor use water and vinegar( weak acid) then dry..then add the oil.

why are you only drain 1 liter? is your titration high enough to require draining? think T14 or more..then is 1/2 the amount the methanol added or 6l not 1l.

-dkenny

ps toss the phenol red..go the store and get some turmeric( a common cooking spice)..its far cheaper and works better then phenol red. I started with phenol red and phenolphtylane(sp)..turmeric is all I've used since 2005..I think I spend $2US on 2 oz...and I'm still using it.


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everything run B100 when its warm enough Smile
 
Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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