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Two Stage Acid / Base Biodiesel RecipesThe Two Stage Acid/Base method is used in commercial biodiesel production to increase yield and reduce soap production. In commercial settings it is used on oil titrating from 2-6 (NaOH). It can be used to make biodiesel from high and very high FFA oils. The process creates water as a byproduct. As the concentration of water increases the reaction is slowed. To combat the slowing of the reaction for high FFA oils, the Acid stage is often performed in steps with the water drained between steps. The most commonly used variation of the Acid/Base method in homebrewing calls for one Acid step followed by one Base step without draining the water between. Precautions
Acids react violently with bases. You will need to take special care to keep your caustics away from the acids. Always add acid to water. Adding water to acids can cause the acids to splash. FATTA RecipeThe internet has a large number of acid/base recipes. The original FATTA recipe seems to be the most commonly cited on homebrew sites. First stage acid catalyst (to esterify the FFA)Oil 1000ml (1 liter) CH3OH 100ml (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 neutralization if titration of 2.6ml achieved) React at 48- 54C for 1 hour. Settle and separate D Kenny’s MethodDkenny is a regular on the biodiesel.infopop.cc forum who regularly uses acid/base techniques. This is his recipe. Throughout he uses KOH titration levels. If you use NaOH to perform your titrations you will need to adjust the formulas accordingly. Acid Stage
Titrate your oil and use the standard 8g + Titration (KOH) to determine your KOH amount for the base stage. If your initial titration was below 14, you will add methanol equal to 10% of the initial oil volume. That would give you 22% total methanol when you add the methanol from the acid stage to the methanol added in the base stage. If your initial titration was above 14, then drain half of the methanol you added for the acid stage before proceeding with the base stage. You will now add methanol equal to 16% of the initial oil volume. The extra 6% is to compensate for the methanol drained. If you drained, remix and recheck the titration. normally it drops from the ending titration Math ExampleOil titrates at 25 KOH60 gallons of oil or 227 liters 25-3 = 22 * 0.2 = 4.4 ml of H2SO4(acid) 4.4 * 227 = 998.8 ml total acid. HANDLE WITH CARE!!!! 12% of 60 = 7.2 gallons of methanol or 27.25 liters In this case the titration might only drop to 7. Let it settle drain 3.6 gallons out Remix and titrate. lets say it reached 3 for the titration after draining for the base stage using KOH 8g (base) + 3 (titration) = 11g per liter 11 * 227 = 2497 grams of KOH total 10% of 60 = 6 gallons of methanol or 22.7 liters If you drained at the end of the acid stage. Add that quantity in additional methanol. In this example since we drained, we would use 6 +3.6 = 9.6 gallons in the base stage mix the KOH in the methanol. Use a sturdy container. it will get HOT!! Add the methanol/KOH to the oil. This is same as a single base only stage. Test for 27/3. Reprocess as needed... Comments
Michael Hall (pressurejet) 16 Aug 2008, 07:56
I have followed D Kenny's recipe 'to the letter' because he seems to be
quite an expert & has much
experience. Please may I ask - in the second stage that followed my acid stage where my lowest titration was 'stuck' on 4KOH after (36 hours) I then started the second stage & the temp increased from 85F to 95F( luckily thro the chemical reaction).Due to the fairly low temp for this second stage how many hours would you process the second stage for before switching off the circulator (pump) & let it settle.Can one process this second stage too long ?
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