I'm going to get this stickied to the top of this forum as soon as I can. IN the meantime, I get email a couple of times a week asking for the recommended acid-base two-stage recipe.

Here's the original FATTA method. This is essentially what I did when I did acid-base.

***************
The FATTA method - Development by Kevin Tidball and Michael Fox
click here for FATTA acid-base method thread from several years ago

First stage acid catalyst (to esterify the FFA)
Oil 1000ml (1 litre)
CH3OH 100m (Methanol)
H2SO4 (conc. 98% 18M) 1-2ml
React at 48- 54C until titration falls to a minimum hopefully 2.6 ml could take longer than 2 hours. Greater levels of acid will raise the titration end point.

Second stage alkali catalyst (transesterification of the oil)
100ml methanol
6.4grams of NaOH
(3.5grams for catalyst + 2.9 grams for acid neutralisation if titration of 2.6ml achieved)
React at 48- 54C for 1 hour.
Settle and separate


Mark

and here is a discussion of the Iowa State University acid-base method. This works wonderfully on very high-FFA oil, but uses more methanol than homebrewers may be used to. I think the exact purity of the concentrated sulfuric doesn't matter0 95% or 98% or whatever, is all OK.

http://biodiesel.infopop.cc/eve/forums/a/tpc/f/629605551/m/933108762

Note that the way they do titration is different than the way we do it- they use more NaOH or KOH in the alkali-water solution than the amount we use.

There's another thread on ways to deal with the extra methanol and the water that is formed in the first stage:

http://biodiesel.infopop.cc/eve/forums/a/tpc/f/629605551/m/585600516

Mark

and here is a place holder 'post' just in case I think of something else meaningful to say before this thread goes off into various directions.

OK, what I really meant to say is:
I want to make this thread a place to send the people who ask 'how is it done?' questions. this spot in the thread is reserved in case someone finds something I overlooked in this forum, which should be a 'basic reference'. If that happens I'll edit this post and stick the forgotten reference here


now, back to welding.

Mark

Girl Mark
I have a few simple questions about the types of aicdic products we use for estfercation #1 What is the best brand names to look for in the case of NaOH this is Draino? So what is the brad name for KOH?
And I was wondering about the use of Pool acid in liquid form that being hydrocloric acid I think I dont have my MSDS with me to give you the exact chimical name but I think you would know what I am talking about. Is Pool acid. Will it work for our process? and has it been tryed ?
Ratski 1996 Ram Dodge 2500 Turbo diesel

HI ALL, I'M A NEW MEMBER. I'M WORKING CONVERTING 100% FREE FATTY ACID INTO BIO-DIESEL. THE MATERRIAL WAS THE SOLID FFA FROM VEGETABLE OIL FACTORY. pH WAS 3.7. I FOLLOWED THE 2 STEP ACID/BASE AND GOT VERY LITTLE (AROUND 1 TO 2%) OF GLYCERIN AND SOME SOAP. THE FINAL PRODUCT WAS DARK BROWN BUT CLEAR. IT STARTED FORMING TINY SOLID FAT DROP AT 26~27 C. WHEN I MIXED 10% WITH DIESEL, THE MIXTURE TURNED CLOUDY AND FINALLY WHITE PRECIPITATION SETTLED AT THE BOTTOM! HERE IS WHAT I DID,
1ST STAGE:
80 ML MeOH, 1ML H2SO4 (98%)
SHAK WELL 5 MINUTES AND HEAT 1 HOUR
COOL OVERNIGHT
2ND STAGE
120 ML MeOH+ 3.1 GRAM NaOH
ADD 60 ML OF METHOXIDE FIRST, SHAKE WELL IN 5 MINUTES AND HEAT AT 55 C FOR 5 MINUTE, SOAP FORMS AT THE BOTTOM, POUR THE OIL INTO ANOTHER FLASK
ADD THE OTHER 60 ML OF METHOXIDE LATER AND HEAT FOR 1 HOUR TO GET THE FINAL PRODUCT

I FOLLOWED MOST STEPS FROM ALEKS' FOOLPROOF. I KNOW THIS IS VERY HARD BECAUSE THE MATERIAL IS FULLY FFA, ANYONE USED TO WORK ON THIS PLEASE HELP! THANKS IN ADVANCE

Where can one get the conc acid? All I can find is %30.

I have followed the foolproof method as described by Aleks. I have a 78 litre processor. My oil titrated at 7.8 using phenal red. I used KOH and did the recommended 3.5 X 1.4 and added 4.90 KOH. After 2 1/2 hours processing stage two I had a fluffy head on the mix. I added 2 1/2 liters methanol and 350g KOH. Reacted for 1 hour and settled 1 day. I had good seperation and drained off the bottom. Added bubble stone and gently washed for 24 hours. Problem now is mixture is murky and holding water. Can this batch be fixed? Must be the water created by the acid, used 93% sulfuric, 78ml. Is the consensus to boil the water off following the first stage? Re-titrate and and adjust accordingly?

Why is it that everyone that tries the foolproof method always asks the same question?

"Can this batch be saved?"

Hello Freetradz, welcome to the forum

Unfortunatly the Foolproof method (Also called the Foolproof joke and the Foolproof Disaster) is total CRAP.
It never makes high quality biodiesel and rarely even achieve seperation.
For the whole hillarious story look Here and Here

Almost ALL the biodiesel information on the JTF site is hopelessly inaccurate and out of date. Some of the recommended prorcedures are just Voodoo nonsence.

[QUOTE]Originally posted by girl mark:
Here's the original FATTA method. This is essentially what I did when I did acid-base.

***************
The FATTA method - Development by Kevin Tidball and Michael Fox
click here for FATTA acid-base method thread from several years ago

First stage acid catalyst (to esterify the FFA)
Oil 1000ml (1 litre)
CH3OH 100m (Methanol)
H2SO4 (conc. 98% 18M) 1-2ml
React at 48- 54C until titration falls to a minimum hopefully 2.6 ml could take longer than 2 hours. Greater levels of acid will raise the titration end point.

Second stage alkali catalyst (transesterification of the oil)
100ml methanol
6.4grams of NaOH
(3.5grams for catalyst + 2.9 grams for acid neutralisation if titration of 2.6ml achieved)
React at 48- 54C for 1 hour.
Settle and separate


I am new to forums so I hope I am asking the question in the right place.

I am tring to make biodiesel using the above recipe.
30 litre batch of 8.6 tritrated Naoh oil
I warmed the oil and added the 100ml/l methanol
mixed well and then added 2 ml/litre sulfric acid. mixed and heated (about 120 to 130 F)until tritration down to 2.2 (3 hours)
cooled and settled overnight.
reheated next day to boil off the water.
cooled and settled.
When I checked the bottom drain I got about 1 litre of black mud and the oil is black. The problem is the oil now tirates at 7.6
Did I do something wrong?
Should I move on to the base stage?

What should I do next?

Thank

quote:

Originally posted by lewis:
HI ALL, I'M A NEW MEMBER. I'M WORKING CONVERTING 100% FREE FATTY ACID INTO BIO-DIESEL. THE MATERRIAL WAS THE SOLID FFA FROM VEGETABLE OIL FACTORY. pH WAS 3.7. I FOLLOWED THE 2 STEP ACID/BASE AND GOT VERY LITTLE (AROUND 1 TO 2%) OF GLYCERIN AND SOME SOAP. THE FINAL PRODUCT WAS DARK BROWN BUT CLEAR. IT STARTED FORMING TINY SOLID FAT DROP AT 26~27 C. WHEN I MIXED 10% WITH DIESEL, THE MIXTURE TURNED CLOUDY AND FINALLY WHITE PRECIPITATION SETTLED AT THE BOTTOM! HERE IS WHAT I DID,
1ST STAGE:
80 ML MeOH, 1ML H2SO4 (98%)
SHAK WELL 5 MINUTES AND HEAT 1 HOUR
COOL OVERNIGHT
2ND STAGE
120 ML MeOH+ 3.1 GRAM NaOH
ADD 60 ML OF METHOXIDE FIRST, SHAKE WELL IN 5 MINUTES AND HEAT AT 55 C FOR 5 MINUTE, SOAP FORMS AT THE BOTTOM, POUR THE OIL INTO ANOTHER FLASK
ADD THE OTHER 60 ML OF METHOXIDE LATER AND HEAT FOR 1 HOUR TO GET THE FINAL PRODUCT

If you use 100% FFA then you do not need a base transesterification step. furthermore, you would not get any glycerin as the fatty acids are free and not bound to a glyceride molecule. Try only acid esterification. What is the source of the FFA? The source will affect the CFPP (clouding at lower temps). Acid esterification may require longer reaction time.

I'm attending the Biodiesel Technology Production Conference in Iowa put on by Van Gerpen & Company.

Thought I'd give the reference for the Acid/Base method which we all talk about.

Jon Van Gerpen did a study in 1999 and in 2001 that was based off of some patents that were filed in the early 1940's that discussed a method for treating feedstocks high in free fatty acids.

In case anyone's wondering, here's the study's.

Canacki, M. and J. Van Gerpen, 1999, "Biodiesel Production via Acid Catalysis," ASAE Transactions, 42(5):1203-1210

Canakci, M. and J. Van Gerpen, 2001, "Biodiesel Production from Oils and Fats with High Free Fatty Acids," ASAE Transactions, 44(6):1429-1436.

The studies measured differences in free fatty acids based on several different levels of methanol, sulfuric acid, and temperature.

-Graydon

For several batches I have been working on a easy way to apply the acid stage. easy to figure and easy to apply. So far I have come up with the following.
First was done using KOH not NaOH. so I no idea if this will work with NaOH.

Take the starting titration
subtract the ending titration, usually this is around 3ml.
Take this result multiply by 0.2ml
then multiply the number of liters of oil
this the total amount of H2SO4 to add.

the Acid is added to 60% of the methanol for the batch.

typically this takes 12-24 hrs for the titration to reach 3ml. sometimes 2.5.

example

initial titration 15ml
final 3
15-3 = 12
12 * 0.2 =4.8ml of H2SO4 per liter of oil
this is higher than other methods!!

I would like to have others that have bad oil to try this and see if it works.
the worst I have used titrated at 18KOH. the method work fine.

there is also no draining of water/gly/methanol
between the acid and base stages.

base stage is done based on the titration only.
no adjustments the acid stage. if the titration ends at 3ml then its 3 + your normal base amount.



-dkenny

quote:

12 * 0.2 =4.8ml of H2SO4 per liter of oil

Hey dkenny,
The last time I checked 12 times 0.2 equals 2.4

So... should we multiply by 0.4?

I had another question, you said to take the starting titration and subtract the final titration. How so we know what the final titration is in the beginning??

Or is the 3 the titration we want to achieve and the numbers would change if we wanted to wind up with...say...5?

Ok is this right if I wanted 5.

15 - 5 = 10

10 x .2 = 2.0

At this point we either have to multiply by 2 to follow your equation or multiply by .4 to begin with. Any way, I'll multiply by two and proceed.

2 x 2 = 4

So it's 4 ml per liter of wvo...Right???


-mcguyver

mcguyver,
yep(to the 12*0.2=2.4 not 4.8). but why would not want the lowest possible titration for the end. typically 3 is the lowest I could reach.
so don't use 4ml/l of WVO it would be too much acid.

thank for the math correction
0.2*12=2.4...use the 0.2ml/l

I have never tried to reach a different ending titration other than 3. so I don't know if it would actually work.

-dkenny

dkenny - is the acid esterification process? It sounds so simple. Just add the sulfuric acid to the oil? It would be great if someone did a step by step rendition of this process. You know, 1. do this 2. do this And list precautions too. My husband and I are panicking because we obtained about 500 gallons of high FFA WVO. 4.5 is not a 'bad' (not that great either) titration, but we're used to very clean .65 (yes .65). After running the acid through, would an additional titration prove the new result so that the brewing process could commence? I'm very concerned about not burning myself or causing a caustic poof in my home lab... still studying in Wisconsin...
Sedona

sedona,
the acid needs mixing with methanol before adding to the oil. the net result is reduction of FFAs in the oil. once the titration(FFA's) is dropped then the normal base process should be used.

-dkenny

ps also note that I use KOH not NaOH so the numbers will need adjusting.

quote:

My husband and I are panicking because we obtained about 500 gallons of high FFA WVO. 4.5 is not a 'bad' (not that great either) titration, but we're used to very clean .65 (yes .65).

sedona,
Are you titrating with KOH or NaOH?? Either way there is no reason to panic. If this titration is with KOH then the cost of doing the acid "pretreatment" is more than the cost of a little additional KOH (Unless your paying an outrageous price for KOH). You have to take into consideration the cost of electricity and acid and all the associated costs. There is a thread where a fellow BDer was comparing the cost of acid esterification verses strait base process. His oil was in the neighborhood of 6 KOH and it wasn't really feasible for him. If you're using NaOH then it is really border-line as to whether it is worth the extra effort to go the acid route. I'd try a couple of mini batches first to make yourself feel more comfortable about doing a regular base or base/base process. If that don't work then perhaps you can do some acid/base testing.

If you want to do the acid/base process, you will need a processor with heat and reasonable sealed to do a good job.


-mcguyver

Thanks for the input! We are using NaOH and are nearing the end of the supply. So, now would be a good time to switch to KOH as I see a lot folks find it dissolves better. NaOH vs. KOH are nearly the same price (about 10 lbs difference for same price). We also have a reasonably priced supply of methanol from a local heating oil company. We get our lye/pot ash from Wausau Chemical in Wisconsin.

We're planning on doing some small batch experimentation based on your recommendation. I've ordered a small quantity of sulfuric acid to run some test batches. We also have a great chemistry equipment outlet in Milwaukee - American Science and Surplus - that I get reagent bottles, flasks, beakers, etc at a really good price. We made the investment in good equipment because we're devoted to this long term. We are heating our home and hot water with B100 and are also using it in our John Deere tractors. This is why we are extra concerned about getting good quality fuel - tractors are more expensive than cars these days and we want to keep them running as long as possible.