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Can someone please walk me through Acid Esterification?
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Hi all,

I am about to do an esterification reaction for the first time, and am hoping to double-check my proposed method with your experienced folk out there.


Background Information

The WVO oil I am using has an FFA of 8%, and required 11ml of 99.99% NaOH solution to titrate (giving it a complete titration value of 16). Also, I have ensured via bubbling that my oil is bone-dry - there is no water in there.

Ideally, I would like the titration to fall down to around 3. However, that is an arbitrary number I've just picked.

Recipe

To make a one-liter test batch:

1 liter of WVO - first heat up to 130F (55 C)
Take 110 ml of methanol, add between 1.5~2 ml of sulphuric acid into the methanol, stirring all the time (95% pure sulphuric acid)
Add the methanol/acid mix into the oil - close container, thoroughly mix
After 4 hours, titrate
Repeat titration every 2 hours until it stops falling

Proceed to normal base transesterification, except only using 110ml of methanol

Questions

Did I miss anything in here? I know I am a complete novice, so if so, PLEASE tell me.

After I mix the methanol/acid mix into the oil, and mix it, can I just leave it - or must I stir it continuously? If I have to stir, won't that allow methanol fumes to come out of the - otherwise sealed - container?

What is the relationship between the amount of acid I put in and the low titration number (3) that I wish to achieve? How can I tell what amount of acid I need to put in for an end number of 3 vs. an end number of 2, for example?

What are the exact precautions I need to take to handle Sulphuric acid? I have read the MSDS - and know I have to wear goggles and gloves. Anything beyond that? Best practices?


Thanks,

Zain

This message has been edited. Last edited by: Zain,
 
Registered: November 12, 2010Reply With QuoteReport This Post
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check your PM Tom


" 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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for handling H2S04....gloves goggles check..
what about a spill?? have any baking soda handy..you should..water?

also know the methanol and H2S04 cause a VIOLENT reaction when mixed...ALWAYS. even if the mixing isn't where you planned..

a couple of comments..might be duplicate from Tom..he and I agree a lot on AE these days..

can you run hotter then 130F..so 160F?? if so do it!
no specific need to mix the entire time..unless you have to mix to maintain temperature..like me..

titration numbers..
for every ml of acid added you will add about 1 ml of titration..when in doubt as the amount of acid. you mention using 1.5-2ml..3-4 mls of titration from the acid alone..this is too much acid for your oil..think 0.75-1ml of acid per liter.. back on track..use less than you think...its easy to add more but impossible to remove!

why does stirring require the vents to be open? if you're not heating close the vents..can you processor handle a small pressure or vacuum? less than 5psi?

-dkenny


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Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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Hi guys,

Thanks for the great advice. I've noted it all down.

Haven't actually done it yet, because my moisture removal solution of air bubbling [so that I can AE bone-dry oil] is causing my major emulsion problems.

Check this thread for more details: http://biodiesel.infopop.cc/ev...1066562/m/6317018323

Help!

Thanks Smile
 
Registered: November 12, 2010Reply With QuoteReport This Post
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quote:
Originally posted by Zain:
Hi guys,

Thanks for the great advice. I've noted it all down.

Haven't actually done it yet, because my moisture removal solution of air bubbling [so that I can AE bone-dry oil] is causing my major emulsion problems.

Check this thread for more details: http://biodiesel.infopop.cc/ev...1066562/m/6317018323

Help!

Thanks Smile


Well for starters:

1) The recommendation of acid esterification is recommended for those oils that have high levels of free fatty acids (more than 5%) that hinder transesterification,

2) You must know what the initial acidity measuring the quantity of H2SO4 to add (titration of the acidity of the oil) so common with KOH in aqueous solution (DKenny)

3) Define the reaction time to lower the acidity.

4) Separate alcoholica/H2SO4/AGUA phase of the organic phase (TGC + metilester)

5) Carry out the transesterification according to conventional methods.
Jorge Zegarra
 
Location: Lima peru | Registered: March 31, 2006Reply With QuoteReport This Post
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