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Summary of the 73 page discussion above
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I am wondering if there is any way to give a general summary of the massive thread above?
It is a very arduous task trying to get meaningful information out of that long and meandering thread, IMO.
Is there a standard formula to give ml/L based on:
1)Purity of HS2o4
2)Titration
3)Treatment done in a dedicated tank vs a combination tank
4)Amount of methanol/L of oil?

So far I have gleaned that you need *dry* feedstock, processing temperatures and constant mixing for good results.
Titrations over 18~20 will require 2 treatments with draining sludge/water in between.
Am I missing anything else?
What about safety? I have read a couple posts stating that adding the methanol to the acid is dangerous and may cause an explosion but I have not been able to dig up any best practices for mixing them together, just that it is safer to add the methanol to the batch first followed by the acid.
Does anybody have a link to a document with best practices for mixing acid with oil and or methanol?
Tom, Dave or whomever may have experience with this, any input here to try and summarize this stuff would be appreciated!
Cheers,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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I see Rick laid it all out pretty clearly over on his great site: http://www.make-biodiesel.org/...id-base-recipes.html
Does this formula still hold true after all of the testing and experimenting in the big thread above?
Milliliters of H2SO4 per liter of oil = (Initial Titration - Target Titration) * 0.2
Methanol needed for acid stage = oil volume * .12
If so I am going to add it to my bio software to calculate it all automatically.
I see Dave recommends adding the acid to the methanol, is there any difference in the outcome of the batch if one adds the acid and methanol into the batch together as apposed to adding the methanol first then acid?
Cheers,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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quote:
one adds the acid and methanol into the batch together as apposed to adding the methanol first then acid?


If you add the acid to the wvo before the methanol is added the finished biodiesel will be a bit darker in colour. I always add the methanol to the oil first and mix well then add the acid.
In the calculation above the target ending titration is 2. Your ending titration will depend on how much acid you use per ltre of oil; whether you drain the junk off the bottom then remix before titration or if you mix the whole lot then do titration. The latter is my preference because it give you a better indication of how well the AE process worked. For each ml of acid/ ltr of oil expect 2 points of titration. So if your titration was 10 to start then you add 1.5 ml of acid per ltr your titration jumps to 13. At the end of the process with all the acid mixed in and you record a titration of 3 you know that all the ffa have been esterified.

I never ever used 12% methanol! I use 8 - 10% of the oil volume. the lower amount at T8 and below and the higher amount up to t15. my oil is mostly in that range.
How much acid should you use? If your oil is dry you can calculate the required amount by multiplying the titration by .085 - .095. Since this process is new to you I would suggest starting at .095 them as you see how well that works reduce the multiplier to .085 then .075. For me this is the only formula I use and get consistent results with a multiplier of .075
be sure to maintain the heat throughout the process, the higher the temp the faster it will work. Buckeye term the phrase high temp AE for processing at the 160 - 165f range. At this temp the reaction will be complete in about 4 hours. at 130F it could take up to 16 hours. at the lower temp you only need to mix for a short time, for your batch size about 1 hour at the higher temp you need to mix continuously.
A separate ae tank is highly advisable. the remaining caustic residue left in you processor and pump/plumbing will cause the outcome of the AE process to be unpredictable.
Good luck and play safe don't mix the acid and methanol together. I had that chit explode all over me, it eat my jeans and the top of one shoe! Not trying to fear monger, alot of people mix the acid and methanol togeather fist. you need a container that as at least 1/2 bigger than the volume of methanol and the acid must be added slowly. Now you are dealing with a huge volume of very acidic material.


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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Thank you for the detailed reply Tom!
quote:
at the lower temp you only need to mix for a short time, for your batch size about 1 hour at the higher temp you need to mix continuously.

With my rig I need to mix continuously in order to have heat as my boiler is inline. If I was to heat to 160f, suck the boiler contents back into the reactor and then start the acid reaction I should be able to mix for at least 4 hours before the temp would drop much below 140F.
That should be fine eh?
I would rather keep the acid away from my boiler if possible as it has a pretty thin skin compared to my reactor and plumbing. The boiler was glass lined but a lot of that chipped away when I customized it lol...
Cheers,
jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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Jon for sure that will work.


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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This acid esterification of free fatty acids is called the Fischer-Speier esterification, first described in the year 1895. You might read up on this Fischer-Speier esterification. There is a lot of information about it on the internet and else where.
 
Location: Texas | Registered: April 27, 2011Reply With QuoteReport This Post



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Thanks guys.
I am going to suck the acid into the reactor just ahead of the pump like I do with the methoxide. That should provide an awful lot of dilution/mixing as it goes in. How slow is slow though, is a litre per 5 minutes too fast? 1L/10 minutes better? Or just suck it in at a steady pace and not worry about it?
When I used to neutralize with muriatic acid ala GL's push/pull, he recommended around 1/2 an hour for only 100ml of acid though that is a different process. I can remember hearing the biodiesel crackle if the acid was going in too fast.
Hopefully soon I will have enough oil for a batch to try this out... Razz
Cheers,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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I just dump the acid in in front of the pump then follow it with about a ltr of methanol to wash out the pipe.
remember play safe, have a box of baking soda and some water close just in case of a spill or splash.


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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Well I gave it a go, though I was somewhat ill prepared it came out pretty good.
I decided to start with fabricators simplified formula of 1ml/L since his setup is very similar to mine.
Started with 1050L of 150F oil titrating 11.5 KOH.
Added about half a drum of methanol, I just eyeballed it cause I seem to have re-purposed my graduated drum from my old reactor. Roll Eyes
I added 1100ml of acid while mixing vigorously.
After the first hour it was down to 8 @ 2h, 7 @ 4.5h it was at 5 and the temp had dropped to 130F so I added the methoxide and started the boiler back up.
After an hour it was up to 155F and it passed with a clear 3/27, I wouldn't call it bright but it was definitely a clear pass. Big Grin The bio is not as dark as I had expected either, for some reason I had it in my head that the bio would be black but its a nice amber instead.
I cleaned out my super sucker by sucking up half a tote of glycerine and then blowing it out. Some must have stayed in there as after I dewatered this batch on Thursday I let it settle overnight and drained about 2 gallons of glycerin out of it. I am sure that didn't help with the acid reaction.
I will be done demething this afternoon and then I will know how my yield is.
Next time I will be more accurate with the methanol and will try Tom's formula.
Cheers,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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Yield = ~950L
I am happy with that Smile
It was a learning experience, next batch will go better...
Cheers,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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quote:
Originally posted by Jon Heron:
Yield = ~950L
I am happy with that Smile
It was a learning experience, next batch will go better...
Cheers,
Jon


Jon,

how much oil did you start with ?

Thx,
John
 
Location: Georgetown, KY | Registered: July 31, 2007Reply With QuoteReport This Post
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1050 litres.
quote:
Started with 1050L of 150F oil titrating 11.5 KOH.

Cheers,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post



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Happy New year Everyone,

Ive been playing around with AE based on BIOTOMs recipe @ .09ML acid.

By Oil is usually around T11 using KOH.

Ive made several 1200L batches without settling/draining between the Acid and Base stages.

This batch, Ive settled for about 8 hours and then drained 4Gal from the AE stage 1.


I am not sure that I see any 'junk' settled out.

Is there a decent way to determine settled Junk vs normal oil? What should the settled
junk look like?

Thanks,

John
 
Location: Georgetown, KY | Registered: July 31, 2007Reply With QuoteReport This Post
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Looks like The Titration is 3.5KOH before draining the 4 Gallons and 2.0 KOH with
the 4 gallons drained.

Any opinions on whether or not I should settle and drain? Is 4 Gallons a good amount to drain?

If this removes water, this may be a good reason to drain.

Thoughts?

Thx, John
 
Location: Georgetown, KY | Registered: July 31, 2007Reply With QuoteReport This Post
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Hi John, I only did one other AE batch since I posted this and I cant remember the numbers but it was successful.
I have since secured better quality oil and have not had to do any AE, touch wood!
Cheers,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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