The FFA recovery equation requires excess acid to achieve the glycerol 
separation. The overwhelming majority of the excess should reside in the 
recovered glycerol/methanol layer. On the other hand, there's apt to be 
a microscopic, perhaps "negligible" amount of phosphoric acid in the 
recovered FFAs. A simple wash would put the kabosh on that.

Todd Swearingen



Keith Addison wrote:

>>Ken,
>>
>>Acid catalysis works well. Industry often uses feedstock of 100% FFAs in
>>order to achieve a "pure" or nearly pure mono-ester  product.
>>
>>The easiest way to test the theory on a pauper's budget is to take the
>>glyc cocktail from two side-by-side trials from identical feedstock and
>>reaction conditions, one a/b and one strictly base, and recover the
>>FFAs. To reduce sample error, larger batches would help, at least a
>>galon or thereabouts.
>>
>>Todd Swearingen
>>    
>>
>
>A question about recovered FFAs from separating the glyc cocktail. I 
>want to do some tests using a/b with high-FFA oil, and I don't have a 
>lot of high-FFA oil. I'm looking for a cut-off point where I'll have 
>to change the method, and ideally I'd like a range of oils with 
>increasing FFA content (up to about 25%), but I'm not going to get 
>that. What I'd really like to do is add FFA by increments to the same 
>low-FFA WVO. Could I use FFA separated from the glyc cocktail for 
>that? Does all the phosphoric acid and all the KOH end up in the 
>bottom layer after separation or will there still be some left in the 
>FFA to confuse the issue? If it's still there in the FFA, could it be 
>neutralised? Any ideas?
>
>Thanks much
>
>Best
>
>Keith
>
>
>
>
>  
>
>>Ken Provost wrote:
>>
>>    
>>
>>>On Dec 30, 2005, at 11:34 AM, bob allen wrote:
>>>
>>>
>>>
>>>      
>>>
>>>>acid/base method for conversion of wvo to FAMEs
>>>>The following is my modification of that procedure
>>>>which works for us, and takes less time, but  requires
>>>>more catalyst.
>>>>
>>>>
>>>>Dissolve 1 ml sulfuric acid in 150 ml methanol and
>>>>add to 1 liter liter dry wvo,  heat to about 60 Celsius
>>>>for one hour.  Then  dissolve 4.9gm NaOH  in 50 ml
>>>>methanol and  add to the reaction mixture.  Continue
>>>>heating for an additional hour, stir for one more hour
>>>>and then let set for 8 or more hours.  Workup as usual.
>>>>
>>>>
>>>>
>>>>        
>>>>
>>>Sounds right -- now as to the basic theory:  Have you
>>>been able to verify that the acid catalysis stage actually
>>>accomplishes anything? In other words, starting from
>>>some high FFA feedstock, do two experiments:
>>>
>>>1) Single stage with excess alkali as required to neut-
>>>ralize the FFAs. This would be expected to produce
>>>much soap and reduced biodiesel yield.
>>>
>>>2) Your method as described above, which should
>>>theoretically reduce the soap formation dramatically
>>>with proportionally higher biodiesel yield.
>>>
>>>
>>>I did my best to verify this a few years back, and found
>>>the acid actually didn't help much. Just curious....
>>>
>>>-K
>>>      
>>>
>
>
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>  
>

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