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Acid Esterification taking 2 treatments
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Here lately I have been getting an average titration of between 15 and 18 KOH. I dump my collection of 60 gallon at a time into a 330 gallon tote.and mix it all together to give me a more consistent tritation value. I always do an acid/base reaction. The recipe I use is step 1 12% methanol titration value less 3 times .2 in sulfuric acid and wait 12-24 hours at 140 degree's in a closed apple seed reactor. The last 10-12 batches I have not seen the titration value drop very much at all 1-3 points. I let it settle and drain the methanol off the bottom (I am sure that I am draining the methanol because it burns my eyes and it is thin like water then 2.5 to 3 gallons later it gets the viscosity of the WVO) and the titration will drop 2-4 more points and. Then I reprocess the acid step with the same acid formula except only 6% the original WVO volume in methanol. Then it drops to a titration of 2-3 KOH. The titration drops are inconsistent with the first step but the second acid step usually gives me the desired result. the base step is usually right on the money with a passing 3/27 test with in an hour and the standard water wash passing the 50/50 soap in 4 to 5 washes(I know that there is room for improvement here but thus is not for now). I am really concerned because I have collected some reasonably better WVO titrating an average of 7 KOH. With the same results as the high titrating WVO requiring a second acid step. The only change in my routine is I have changed to KOH from NAOH. I don't think my titation's are inaccurate because my base step seems to be perfect passing the 3/27 almost every time with only 1 base reprocess in the last 10 batches. The base process is consistent with the NAOH processing times. I have the same supplier of sulfuric acid also. Can anyone point where I may be in error? What would be the effect if I changed my multiplier for the acid formula from .20 to .35 or .40 maybe? Oh yea my average process is 48 gallons 22 liters of methanol step 1 if titration is 15 I multiply 15-3 = 12 12 X .2 = 2.4 2.4 X 182= 440 ml of sulfuric acid mix with methanol and slowly add to WVO. @140 degree's 12-24 hours let settle 6 hours and drain the methanol acid off bottom and titrate add back usually about 10-12 liters of methanol and acid then on the second acid step I can usually titrate every hour and watch it drop about 1 to 1-1/2 points every hour.
 
Registered: August 30, 2008Reply With QuoteReport This Post
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marvingvx

-you have a water problem FOR SURE. your wvo is not dry enough With your T 18, you should be able to squeek by with one acid treatment, but the wvo will have to be bone dry. put the wvo through the same drying proceedure that you use for drying biodiesel. 5% water by weight will reduce the esterficatiom of ffa"s by 85%. seems to me thats your situation. Tom


" 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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I'm sure that may be possible but my drying process is 12 hours(cut the heater on before I leave work and let it cook until the next morning) at 230 degree's. A quantitative water test. I weigh the WVO and boil it on the stove with very little bubbling with usually less than .2 % loss on weight I an aware that some say .05% and others have said that 1% is good enough. My goal is .5% or less. In the past with a base only reaction early in my learning I have had water kill my batches how come the water doesn't affect my base reaction? Is it possible that I am removing some of the water when I am draining the step 1 methanol draining? I dont filter my oil very well. I see the trash (carbohydrates? FRENCH FRIES,CHICKEN CRISPIES AND BREADING) settle out with the gly.
 
Registered: August 30, 2008Reply With QuoteReport This Post
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I don't see anything about the acid wvo mix being circulated for any length of time. I wouldn't think there would be any noticable methanol to drain off using 12% methanol to the wvo volume . Its not like an overdose rate just a little over half the normal rate between the two stages.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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Marvingvx
-.2%, is 2000 ppm, away too high for acid esterfication. you can get away with base transesterfication with that water content,( ae is much more water sesative) but the high ffa will reduce the yied to about 50%, and make a great amount of soap. You don't need to heat the wvo beyond 150f, but it needs to be adgitated in some way to drive off the water vapour. I pump the wvo from the bottom of the tank and spray it back in the top, it takes about 24 hrs to get it dry enough for the ae treatment. Tom


" 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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heatbeater

-if the esterfication fails to take place, then the methanol/water/acid will be on the bottom, the methanol will not stay in the mix in this case. to see this, place 3 ml of wvo in 27 ml methanol, shake the crap out of it and see what happens. Tom


" 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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I tried the low heat and circulating in a tote a couple times over the weekend and had a few cars I had to clean it covered every car in the shop with a film of oil LOL can't do that any more. So until I finish the new gl processor this is the only way I have to dewater. I have noticed in these batches as of late that when I drain the step 1 methanol that the first liter or 3 looks like mud before the thin methanol starts to flow. I guess this is food particles where most the water is? My yield is about 80-85% after wash is done. Could the acid be neutralizing the food particles or visa versa ? If this is the case would if be OK to process in the manner that I have accidentally seem to have stumbled upon? Passing the 50/50 soap test and the 3/27 with an 80%+ yield until I have new processor. Or Is there something that I am not considering? Also I have a dewatering Idea that I am designing. It's a cold upflow system including a 55 gallon drum and 2 275 gallon totes. I try to process 3 50 gallon batches a week so volume is necessary. Averaging 120 130 gallons a week of finished product. Hoping to double this with new processor.
 
Registered: August 30, 2008Reply With QuoteReport This Post
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Marvin,
A contributing factor may be your water heater not allowing full draining of the water/ acid mix after your first acid stage.
Since Sulfuric is highly reactive with organic compounds, it wouldn't be surprising if some of it were consumed by the food particles.
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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marvingvx

-the mud is another indicator that you have a high water count. I am surprised that your yield is that high. if this works for now, I think it's the best you can expect. once you have a system in place to properly dry the wvo, you can expect yield to increase to 98-100% Tom


" 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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Originally posted by Double D:
Marvin,
A contributing factor may be your water heater not allowing full draining of the water/ acid mix after your first acid stage.
Since Sulfuric is highly reactive with organic compounds, it wouldn't be surprising if some of it were consumed by the food particles.
Yes this is probably true. I transfer to a cone bottom settling tank to drain but processor eats heater elements about every 8-10 batches. I have to change an element and vacuum out the sludge that gets up to the element. This project has been an evolving project for me and I have just learned a significant piece of information from you all. thanks D and Tom
 
Registered: August 30, 2008Reply With QuoteReport This Post
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Originally posted by Biotom:
marvingvx

-the mud is another indicator that you have a high water count. I am surprised that your yield is that high. if this works for now, I think it's the best you can expect. once you have a system in place to properly dry the wvo, you can expect yield to increase to 98-100% Tom
This 98%and 100% thing I have seen several people posting I have a hard time comprehending. If you are removing mono , di, and triglycerides. How can you remove a volume of mass and still retain the same volume? Is the methanol transformed into the esters of the bio diesel? I don't know much of this yet. I haven't done much research into demething so this may become clear in this phase of my education. But 100% almost seems unrealistic even with a pristine VO.
 
Registered: August 30, 2008Reply With QuoteReport This Post
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marvin
-are you pulling my leg? yes, 12.5% or there abouts of the methanol is converted into esters. the ffa's are converted into biodsiel, so 100% is possable if the wvo is clean and super dry before you start. starting with T 10 wvo I routinely get yields above 95% useing ae/base/base process. Without AE, yield is around 60% Tom


" 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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I kinda suspected this but I have to prove stuff to myself. I started with an Appleseed reactor with a lot of flaws in the design. Now that I have worked a lot of the problems (and have learned a lot about the hows and why's of each step in the process as a byproduct of learning about the design flaws) out. I am building a redesign reactor with a lot of changes that I have learned along the way way. I just haven't learned the in-depth knowledge about the trans esterfication process as to the maximum yield and there is I am sure a multitude I have still yet to learn Tom thank you very much for imparting your knowledge on this forum.
 
Registered: August 30, 2008Reply With QuoteReport This Post
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Marvin
-no problem, I got all my info from this great site, and I'm here to repay a debt! (on the threads or by PM) Just seems there have been several tilly cones the past several weeks, and I don't like to get sucked in. Not that I don't have the utmost respect for that persons knowledge, But I don't support the antics of late Tom


" 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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LOL If I'm a Tilly clone I must have set it up a year ago.HA HA HA HA But I know how you probably fee l I didn't like the way that he belittled biogirlz and some other people with his clone users thanks again Tom
 
Registered: August 30, 2008Reply With QuoteReport This Post
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marvingvx,

sound like you're on the right track but running into the usual stumbling blocks to AE processing.

1. water - in AE stop the conversion..remember we are making BD during this stage. during base processing oil, water, caustic...these make SOAP! during the acid stage it only stops the process.NO soap is made

2. for drying..think about how you dry your finished BD? for me I spray,heat and bubble..I only get my oil to 130-140F during this stage but it might take 2 days to complete..

3. filtering the oil..through a window screen is good enough..all large chucks are caught.

listen to Biotom..and read the thread( 27+pages) on the call for acid/base users that I started..you'll learn alot..

don't increase the multiplier..0.2 has already been shown to be TOO much..

now with all that said..are you stuck in the middle of batch that's not working? in this case adding more methanol/acid might push the process.

if you're starting at T18..you should see a drop to atleast T7 before draining..

-dkenny


'84 bluebird school bus, DD8.2L turbo( 4/2011, the bus tranny has died..Frown 8.23.11 bus driven to scrap yard Frown )
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Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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-dkenny I see I should stay with .2 until I improve my process. If my titration doesn't drop below 7 should I just add more acid until I get it below 7 or should I add more methanol also and if so what percentage? I would assume that after the titration stops dropping that I use the standard .2 multiplier of titration -3. What I have been doing in the case where the t doesn't fall much is settle,drain,and add the amount of methanol I drained subtracting the approximate amount of mud that was removed plus the .2 formula X titration -3. As a side note With WVO I don't cull anything within reason. This is why I mix all my oil so I have an average titration instead of a t of 22 for 1 batch and t of 7 for next batch.My average is usually lower than this until recent collections. Reason is I picked up a couple new accounts and my driver sucked the bottom out of there WVO thanks. they must have been rancid from being a long time since last collections. I do not have any sludge byproduct to dispose of just some lumps in the gly after the 2nd or 3rd stage separation. Except for the mud that comes out with the acid meth drain after the 1st acid stage.
 
Registered: August 30, 2008Reply With QuoteReport This Post
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I tried doing AE on two batches by adding the acid first and blend than the methanol it didn't work. This last batch I mixed the acid with methanol than blended just like doing a base reaction and the titration was cut in half in 6 hours. Now I can't see how in can work by anding the acid and methanol separately, we don't do it that way for the base reactions. I came up with a factor of .3 using 250 ml. of Rooto on 170 liters of wvo and a titration drop of 5.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post



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Marvin

Biotom and DK are correct when they talk about the water affecting your final T and yield.
My oil is consistantly at T 15-18,some higher. The last batch I did about 3 weeks ago yielded a 100% bio to oil ratio. The two things I changed was filtering to a 1 micron @ a low transfer rate and dewatering my oil till it was super dry. I took the top off the appleseed and left the pump and heater(145) on for 24hrs. No bubbles at all in the pan test. Using a multipler of .15acid I achieved a final T of 3 in 16hrs.

Before changing these few items in my process I was having the same problems as you have mentioned. Final T's not below 6 final yields anywhere from 45 to 95%. It was always a crap shoot to see how much Bio I would get on each batch(no consistancey what so ever)Hope this helps. Good luck.Going to start a new batch in the morning useing an even lower multipler.


jrunlimited
 
Location: Texas | Registered: June 15, 2008Reply With QuoteReport This Post
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I'm not sure what the difference in the process I am doing but I consistently get 80%+ out of my WVO. I know I need to change my drying process. That isn't an option right know at least for a few weeks down the road I have a steady stream of WVO that has to be processed. I would like to know to know if there isn't enough acid to complete the process is it better to add the acid raw or is it better to mix with more methanol. and Thanks so much for your response guys
 
Registered: August 30, 2008Reply With QuoteReport This Post
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