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Here is a comparison of my normal batches to the “demeth the whole batch” method.

First a little background on my regular processing procedure:
*75 lt batch with a GL-1 reactor
*Home made venturi
*Plumbers delight condenser
*18 gpm pump
*90% KOH
*22% methanol
*2 stage base/base (80/20)
*Average T of 7
*WVO is partially hydrogenated canola
*1st base ran for 1 ½ to 2 hours
*2nd base ran until passes 3/27 (45 min to 1 hr)
*Total glycerin 18-20 liters
*Recovered methanol 1 ½ to 2 liters
*Yield 90% to 95%
*prior batches:
Batch 1 (3batchs/50gal) settled 3+ weeks in 55 gal barrel = 670 ppm soap.
Batch 2 settled 1 week in 5 gal buckets =509 ppm soap.
Batch 3 settled 24 hr in 5 gal buckets = 506 ppm soap

First WBD batch processed the same as previous batches. Recovered 3.7 lt methanol and approximately 20 liters of by-product. Yield was only about 85%. Soap content right after drain processor was 917 ppm. I will test it again in a couple days after it settles and post the results.

Isn’t the 12.5% figure in the stoich formula with ALL the bi-product remaining? So if you do a 2 stage base/base wouldn’t a lot of the calculated methanol be drained off in the first stage? If I understand this right, you would be draining off to much methanol when doing the WBD after the second base stage and risking reversal.

Tim
 
Location: Central Oregon | Registered: 17 May 2008Reply With QuoteEdit or Delete MessageReport This Post
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Hmmm, interesting, your first wbd batch soap was very close to mine.
 
Location: West Michigan | Registered: 26 April 2006Reply With QuoteEdit or Delete MessageReport This Post
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It's probably my description not being too clear, so you probably got some reversal there then Jon as took 500ml too much, 12.5 litres needed + 9.5 Recoverable = 22% start amount.

If we take the average stoich amount for the majority of oils/fats as 12.5%, then we can recover anything over and above that amount without taking what is needed for the bio, the guide shows what the stoich amount is for the batch size when using 22% methanol, the other column is what you can safely recover, going further can cause reverse reaction, most like to stop 500ml or so short and bubble off any residual meth once the glyc is drained to be safe.

Since getting such good purity methanol back I now use 25% methanol as it's easier to work out the recoverable amount being just under half.


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Location: S.E. England | Registered: 05 September 2004Reply With QuoteEdit or Delete MessageReport This Post
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quote:
Originally posted by fabricator:
quote:
Originally posted by Eurocab:
Fab,

Congratulations on your results. Perhaps you could start a thread outlining your method of filtering the BD on the drywash section. Wink

Thanks Chug, for starting this thread.


All I do is cold down flow, then fuge it for 12-16 hours till it is almost clean enough to go back in the fryer, and bone dry.


Fab,

You fuge for 12-16 hours continuously? I guess since you're not pulling out soap but rather particulate matter, the heat isn't a concern?? Please expand on this conundrum...
 
Location: Little Elm, TX | Registered: 12 December 2007Reply With QuoteEdit or Delete MessageReport This Post
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As far as yield... my yield went down. However I will disclose that I used a base/base 2 stage reaction and the WVO wasn't dewatered to make sure it was bone dry. That could be why I lost yield if some of the oil and trace water combined with lye to make soap and caused the first round failure of the 3/27 test.

Dewatering has become something that I think is out of reach for me using a water heater. One of my upgrades when I build processor 2.0 will be a cone bottom tank which will allow for heat and settling and draining the bottom of the batch prior to reaction.

I had a big soapy mess in the tank that I transferred the batch to. Somewhere between the transfer and completing the 3hr circulation to drive off trace methanol, a BUNCH of soap landed at the bottom of the barrel.

All in all I think I converted 26 gallons of WVO into 22 gallons of biodiesel. I feel like I'm playing in the little league sandbox with these small batches.
 
Location: Little Elm, TX | Registered: 12 December 2007Reply With QuoteEdit or Delete MessageReport This Post
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TeePee,
Just my 2 cents and I have not done this yet but I would think if you want to do a 80/20 base/base recipe then you should do what others do with the 5 % prewash... after you pass your 3/27 add all the 1st stage glycerin back in then do your WBD as everyone else is doing.. once added back I would think it would be the same as if you had done 1 stage and never drained..

Just a thought



Lisa 2006 Ford F250 6.0L Powerstroke with 12 inch lift


 
Location: TX | Registered: 20 August 2008Reply With QuoteEdit or Delete MessageReport This Post
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Just curious. What's the point of doing an 80/20 split anyway if you plan on reclaiming the majority of unused methanol? I thought the split was to try to get methanol amount down but reclaiming it all defeats the purpose of trimming methanol from the process.
 
Location: Little Elm, TX | Registered: 12 December 2007Reply With QuoteEdit or Delete MessageReport This Post
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quote:
Originally posted by PwrStrk6spd:
Just curious. What's the point of doing an 80/20 split anyway if you plan on reclaiming the majority of unused methanol? I thought the split was to try to get methanol amount down but reclaiming it all defeats the purpose of trimming methanol from the process.

some still process with the normal amounts of methanol and koh.. the purpose is simply because you get an easier much better conversion. When you use 22%meth and normal koh it is so easy.

If I could reclaim my methanol I would definitly use 22% meth on a base/bsae recipe. I only use less to save money..



Lisa 2006 Ford F250 6.0L Powerstroke with 12 inch lift


 
Location: TX | Registered: 20 August 2008Reply With QuoteEdit or Delete MessageReport This Post
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The glycerine in the batch causes an equilibirum a little higher than 80% conversion. Also when it gets to a point so much of the methanol just dissolves in to the glycerine. By draining it off then reacting again the concentration of reactants to products is again high leading to higher and faster conversion.. as the reaction goes two way, removal of the glycerine prevents it going the wrong way
 
Registered: 02 March 2009Reply With QuoteEdit or Delete MessageReport This Post
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quote:
Originally posted by Reece123:
The glycerine in the batch causes an equilibirum a little higher than 80% conversion. Also when it gets to a point so much of the methanol just dissolves in to the glycerine. By draining it off then reacting again the concentration of reactants to products is again high leading to higher and faster conversion.. as the reaction goes two way, removal of the glycerine prevents it going the wrong way


thanks Reece.. now I know more!



Lisa 2006 Ford F250 6.0L Powerstroke with 12 inch lift


 
Location: TX | Registered: 20 August 2008Reply With QuoteEdit or Delete MessageReport This Post
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quote:
I hesitate to post those results, but there it is on the sight tube.


Goes to show the difference between understanding and observation. They do not always agree. One or the other needs adjusting. Usually the understanding gets adjusted, unless the observation was a measuring error. Wink


Andrew

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Location: Northern California | Registered: 27 February 2006Reply With QuoteEdit or Delete MessageReport This Post
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quote:
Originally posted by PwrStrk6spd:
quote:
Originally posted by fabricator:
quote:
Originally posted by Eurocab:
Fab,

Congratulations on your results. Perhaps you could start a thread outlining your method of filtering the BD on the drywash section. Wink

Thanks Chug, for starting this thread.


All I do is cold down flow, then fuge it for 12-16 hours till it is almost clean enough to go back in the fryer, and bone dry.


Fab,

You fuge for 12-16 hours continuously? I guess since you're not pulling out soap but rather particulate matter, the heat isn't a concern?? Please expand on this conundrum...


No, when drying oil the heat is something you want, I heat to 170 degrees when I'm drying/cleaning oil.
 
Location: West Michigan | Registered: 26 April 2006Reply With QuoteEdit or Delete MessageReport This Post
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quote:
Originally posted by Chug:
you probably got some reversal there then Jon as took 500ml too much, 12.5 litres needed + 9.5 Recoverable = 22% start amount.

DOH! Roll Eyes
Well I guess I screwed that up eh! Not much point in doing the phlip now as I have exceeded the recoverable amount...
I am not to keen on trying this again as its just too easy to add the acid and not have to worry about the stoich... That being said the more I think I am understanding what this stoich represents the more I am thinking it is probably just as important to not exceed it even when using acid to neutralize the caustic?
Does anyone know if the bio will back react with glycerin without the caustic involved?
Where can I do more reading to help me understand the stoichiometric situation? Big Grin
Jon
 
Location: Wellington County, Ontario Canada | Registered: 07 February 2008Reply With QuoteEdit or Delete MessageReport This Post
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quote:
Originally posted by Jon Heron:
Where can I do more reading to help me understand the stoichiometric situation? Big Grin
Jon


Hey Jon,
I made up this excel spreadsheet a while ago based on my WVO. Its typical canola/corn blended cooking oil.

Also these calcs were based on the assumption of 100% conversion in one reaction.

I agree, it seems much easier and safer to neutrolize catalyst first

Excel Spreadsheetstoic.xls (19 KB, 31 downloads)
 
Registered: 02 March 2009Reply With QuoteEdit or Delete MessageReport This Post
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I guess I need to get a bit more edumacation on stoichiometrics too. I can't even spell the word. Red Face

I had no idea that different oils would consume different amounts of methanol upon conversion. I guess it makes sense though.

Jon,

quote:
Does anyone know if the bio will back react with glycerin without the caustic involved?


I guess anything is possible, but the whole idea of the push/pull using acid was to prevent back reactions from happening. I don't see how it is possible for the homebrewer.

You might as well give it another try, since you have the testing kits. Just stop short of recovering too much methanol. I would do it if I had my recovery system together. I just can't seem to get motivated. Frown
 
Location: Chambodia | Registered: 31 December 2007Reply With QuoteEdit or Delete MessageReport This Post
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Big Grin
Hey I just emptied my reaction vessel and performed a much more accurate measurement on the recovered methanol, if it was any closer to 9.5L it would be off!
So the experiment is still on!
Reece,
Thanks for the spreadsheet but I am afraid that I need to do some more research before I could even pretend to know what is going on with it! Smile

Eurocab,
quote:
I don't see how it is possible for the homebrewer.

Which part? the neutralizing? If so why dont you think its possible?
Jon
 
Location: Wellington County, Ontario Canada | Registered: 07 February 2008Reply With QuoteEdit or Delete MessageReport This Post
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haha unless you do spreadsheets yourself i agree its hard to follow others workings..

basically i calced I use 11.9L of the 20L I use. Just made it up so i could approximate how much meth i could recover from my glycerine and biodiesel
 
Registered: 02 March 2009Reply With QuoteEdit or Delete MessageReport This Post
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Smile I can program you an app in C++ or assembly but my experience with excel could be written out on the head of a pin!
Where did you get the values or the formula to calculate this?
I learned more than I cared to know about the definition of stoichiometry HERE but I am still not sure how one would calculate it for our application or better yet what to punch into your spreadsheet to get what I need...
Jon

Yesterday I couldn't spell chemist and now I are one... Big Grin Big Grin LOL
 
Location: Wellington County, Ontario Canada | Registered: 07 February 2008Reply With QuoteEdit or Delete MessageReport This Post
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quote:
Originally posted by Jon Heron:
Here is a pic of the 2 samples settling/evaporating methanol. The one on the left is the pre, you can see it is slightly clearer then the post but they need to settle for a week or 2 to be sure. If you look just right at the post sample it looks like there is a soap structure suspended in the bio so once the remaining methanol evaporates it may settle out but time will tell...
Jon
 
Location: Wellington County, Ontario Canada | Registered: 07 February 2008Reply With QuoteEdit or Delete MessageReport This Post
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quote:
Originally posted by Jon Heron:
Smile I can program you an app in C++ or assembly but my experience with excel could be written out on the head of a pin!
Where did you get the values or the formula to calculate this?
I learned more than I cared to know about the definition of stoichiometry HERE but I am still not sure how one would calculate it for our application or better yet what to punch into your spreadsheet to get what I need...
Jon

Yesterday I couldn't spell chemist and now I are one... Big Grin Big Grin LOL


After reading this I had to open the xcel sheet, even though I'm on dial up. Smile
Reese, I totally agree it's very difficult to understand if your not the one that created it. I work with excel everyday and still don't know where to start. Don't worry though, I created one a couple years ago that I doubt anyone but me would understand. I created mine with a cell to input the starting titration and oil type that would give me everything from the amount of acid to use in an esterification to the base and methanol qty in Neutrals base/ base formula. Then that computer died and I have yet to recreate the sheet. It looks like a good one though, if you understand it. Smile
 
Location: central virginia | Registered: 13 March 2008Reply With QuoteEdit or Delete MessageReport This Post
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