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Biodiesel from cracked Glycerine byproduct
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I’m relatively new to the art of making bio diesel and now have amassed several cubies of Glycerine by-product, which are now taking up space in my workshop area. I’m loath to send them to the land fill etc and I have no interest what so ever in making soap out of it. But on the other hand if one Acid cracks the by-product one gets relatively pure Glycerine and FFA (the soap made from FFA during the base stage turns back into FFA) in roughly equal measure and a bottom layor of salts.

Now is it possible to take these 100% FAA's and perform acid esterification on them with methanol to convert them directly into yet more Biodiesel. And Bypass the base stage as the glycerine has already been removed and go straight to a wash cycle. Am I missing something here or is everyone literally throwing away perfectly good fuel in the form of un-recovered FFA’s. I got some conc. H2SO4 to perform acid base experiments ill give cracking by-product a go and see if i can make Bio from FFA over Christmas, watch this space.


VW Passat 2.0 TDI with a BKP engine 86,000 miles on B100 and not going strong. Bio-diesel broke oil pump drive shaft! ..No oil pressure, dead turbo.
 
Location: Calne, Wiltshire, England | Registered: October 22, 2008Reply With QuoteReport This Post
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Yes, I have done a lot of this- it works really well because the recovered oils are so water-free to begin with, and because esterification of FFA's in biodiesel (that's what you have in the 'oil' layer) is a lot easier than esterification of FFA in triglycerides for various reasons.

Mark
 
Location: Pittsboro, North Carolina | Registered: March 07, 2001Reply With QuoteReport This Post
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Thanks Mark great to know it will work before i try it. i wonder why its not standerd practice. if it works well i think i will start reprocessing other bio producers glycerine waste.


VW Passat 2.0 TDI with a BKP engine 86,000 miles on B100 and not going strong. Bio-diesel broke oil pump drive shaft! ..No oil pressure, dead turbo.
 
Location: Calne, Wiltshire, England | Registered: October 22, 2008Reply With QuoteReport This Post
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People tend to be afraid of esterification, because with oil/FFA mixtures it's less predictable than transesterification. Also, it introduces another very nasty chemical to work with and store.

Also, neutralizing crude glycerine (to extract FFA and biodiesel) isn't all that safe either. You're handling strong acids.

Cracking the soap in glycerine byproduct also requires strong acids, and if you're using sulfuric and other very strong acids, you can get violent boiling and the possibility of acid being spit back out at you in the container when you add the acid to the initial crude glycerine .Be very careful please. Hydrochloric causes other issues but tends to be more dilute so it doesn't boil the glycerine.
 
Location: Pittsboro, North Carolina | Registered: March 07, 2001Reply With QuoteReport This Post
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And whatever you do do NOT mix nitric with sulfuric into the glycerine layer. That is the recipe for Nitro Glycerine in it's most unstable form.



** Biodiesel Glycerine Soap - The Guide
- on 5 continents helping people make & sell soap from the Biodiesel Glycerine.


 
Location: :-) Great White North eh ? | Registered: December 10, 2004Reply With QuoteReport This Post
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Thanks for the words of caution, i hadn't anticipated a violent reaction witout water being present. i'll look at doing the mixing in a covered environment. Any idea how many ml of acid I should use per litre of by-product its 98.8% strength..


VW Passat 2.0 TDI with a BKP engine 86,000 miles on B100 and not going strong. Bio-diesel broke oil pump drive shaft! ..No oil pressure, dead turbo.
 
Location: Calne, Wiltshire, England | Registered: October 22, 2008Reply With QuoteReport This Post



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alcohol also makes sulfuric acid heat up and therefore you'll get boiling. Doing it in a closed container, or stirring, both take care of the problem.

Do a soap test (titration) using a sample of glycerine, the acid you're cracking with (cracking is not the right term, of course) and some bromophenol blue as the indicator. I do this in isopropyl alcohol as the solvent for the titration.
 
Location: Pittsboro, North Carolina | Registered: March 07, 2001Reply With QuoteReport This Post
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sorry, that wasn't very clear

what you do to figure out how much acid to use is to do a titration where you add acid to a sample of glycerine in isopropyl alcohol and bromophenol blue indicator. It'll tell you how much acid to use.

The exact proportions needed to make the titration readable depend on the strength of the acid.

I havne't done this in months so I can't recall what amounts I used- something like 10 ml glycerine, in enough isopropyl alcohol so that you can see the blue color of a squirt of bromophenol blue. It'll take something like 1.5 ml of 32% hydrochloric acid but of course the exact amount will depend on the soap levels of the glycerine. I might be totally misremembering the proportions though.
 
Location: Pittsboro, North Carolina | Registered: March 07, 2001Reply With QuoteReport This Post
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Thank you have been most helpful, I'll keep you posted on how it goes. I guess one reason it may not be popular is if one has to use a lot of acid. If so it no longer becomes cheap fuel, where I’m getting my acid from its about £10 for a litre. Admittedly I’m getting it from a lab supplies company. Where I’m getting my methanol and caustic I get a killer deal, but unfortunately they don’t’ sell acids. Perhaps I should approach in industrial chemical supplier. I’m currently using the acid to add to my wash water. Before I started using it I’d lose about 5-10 Litres of bio from an 80L batch during the washing process, now I recon I only lose about 250mLif that throughout the entire wash process. Most of the product seemed to disappear on the first wash I guess it was instant soap formation when the water was added. I never had emulsion problems though just a lot of soap washing out (grey water). May be I’m adding to much caustic, on the other hand I do the 27/3 test on each batch and always get complete reaction, I’m using 22% Methanol in order to drive the reaction to completion. I don’t like the idea of any mono or diglycerides in my engine.


VW Passat 2.0 TDI with a BKP engine 86,000 miles on B100 and not going strong. Bio-diesel broke oil pump drive shaft! ..No oil pressure, dead turbo.
 
Location: Calne, Wiltshire, England | Registered: October 22, 2008Reply With QuoteReport This Post
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Are there any step by step instructios for "cracking" glycerol by product?

Thanks, Dana


Dana Knight "dckfly"
Boulder, CO

Chevy Silverado Duramax
3 VW TDI (wife and friends)
 
Location: Boulder, CO | Registered: May 13, 2007Reply With QuoteReport This Post
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