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Hi Tom, My starting titration was 11, we added 11 Litres instead of 1.1 litres, we added methanol this morning and will mix with heat for about 4 hours, then see what it looks like. At the moment it is very dark (black) in colour. Jim.
 
Location: Cape Town | Registered: May 17, 2006Reply With QuoteReport This Post
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Jim,
If I were in your shoes, I would want to drain as much of the sulfuric as possible before going into base processing. After settling, drain until you reach oil. The phase change will likely be hard to distinguish. If your processor is allowed to cool the change in viscosity is the best indicator. In case you can't see the phase change, it should be close to the original volume of methanol that was used.
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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Hi DD,thanks, yep dropped out as much as was put into the original WVO very H2S stinky, now added methoxide and processing, if all goes according to plan I expect we will end up with very dark bio. Lets see. 4 years + into making Biodiesel, and still learning.
By the way the T dropped to 3.5, so some good, hopefully, happened.
 
Location: Cape Town | Registered: May 17, 2006Reply With QuoteReport This Post
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3.5!
Not bad at all Jim.
One consideration to ending titration is that the methanol, sulfuric, and water are completely miscible. Just like water in oil doesn't settle out completely in that short an amount of time neither will all the water, sulfuric, and methanol. Some of what your reading in the T 3.5 is sulfuric. It's hard to tell how much, either way the FFA level is actual lower than the titration indicates. Your caustic amount to use is still base + titration but your yield may be a bit higher than if the titration was only reading FFA.
If you would, let us know how the yield turns out.
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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If bringing the T down to the low figures of say virgin Oil or near with AE, then will the BD have better CFPP.
Is the value of the T proportional to the CFPP temp?
ie. the T of the Oil is proportional to the CFPP
Thanks
 
Location: Meath | Registered: November 26, 2007Reply With QuoteReport This Post
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quote:
Originally posted by djc:
If bringing the T down to the low figures of say virgin Oil or near with AE, then will the BD have better CFPP.
Is the value of the T proportional to the CFPP temp?
ie. the T of the Oil is proportional to the CFPP
Thanks


The two are not related no.
 
Registered: February 25, 2010Reply With QuoteReport This Post



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quote:
Originally posted by BWilder:
quote:
Originally posted by djc:
If bringing the T down to the low figures of say virgin Oil or near with AE, then will the BD have better CFPP.
Is the value of the T proportional to the CFPP temp?
ie. the T of the Oil is proportional to the CFPP
Thanks


The two are not related no.

Agreed, the titration result is not really linked to the CFPP temperature.
 
Location: East Yorkshire | Registered: January 14, 2006Reply With QuoteReport This Post
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Reviewing this thread for the umpteenth time it is apparent that the lower acid amount I have been preaching does not give good results to everyone on all batches. Water content of the oil and caustic contamination in the processor are two big factors contributing to AE failure. Can this be overcome? Is there an acid amount that could be used that will help mitigate the effects of wet oil and caustic contamination?
This past summer it was so humid that drying the wvo became very difficult and onerous, “need to find a better way” in addition the quality of my oil supply has greatly deteriorated now it is between T16 and T20 NaOH . I Have since increase the acid amount to 3 ml per ltr of oil, methanol is the same at 10% with the remaining 10% saved for base processing. What this increased acid amount has done is forced a portion of the methanol laden with water and acid to the bottom of the processor. I can drain off about 5 ltrs of this mixture before oil starts to drain. (this amount is replaced with new methanol for base processing) The resulting titrations have averaged 1.5 NaOH and the following base process has been outstanding giving yields of 98 – 100% of the original oil volume.
The AE process was simple, heat the wvo, add the methanol, mix for ten minutes then carefully add the acid, mix for three hours then let settle over night, (heat on) drain, mix then titrate. 12 batches in a row, no flops so I thought I would share. (batch size 160 ltr of wvo) 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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Stir for three hours? Doesn't this much stirring result in a poor reaction?
Shouldn't you just stir for a few minutes and then let it sit with the heat on?
quote:
Originally posted by Biotom:
The AE process was simple, heat the wvo, add the methanol, mix for ten minutes then carefully add the acid, mix for three hours then let settle over night, (heat on) drain, mix then titrate. 12 batches in a row, no flops so I thought I would share. (batch size 160 ltr of wvo) Tom
 
Registered: October 04, 2010Reply With QuoteReport This Post
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The reaction, as shown by the ending T is not affected by the 3hr stir. I may be able to cut down on that time, and I will experiment once the biodiesel demand slows down at the end of this heating season. 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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Well, I tried using some reclaimed methanol for my acid step this go round. It did make a big difference in my numbers. start T 5.2ml NAOH end T 2.2 ml NAOH. The last 5 batches have been right at either 1 or 1.1 ml naoh. The only other thing that could have affected it was that I left my vent open on the processor, which I usually never do. I think I may opt to neutralize this batch just make sure my processor is not got leftover caustic. This is such a learning process. Thanks to all again for all this info on the acid step.


powering
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Location: morgantown wv | Registered: June 18, 2008Reply With QuoteReport This Post
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RR how much acid did you use/ltr of oil?


" 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 haven't been back to the lab yet to get those numbers, but I've been using the .18 multiplier It was 1070 ml in 375 gallons of oil with 35 gallons of methanol. Batch still did ok. my yield was about 370 gallons of fuel before demething. I decided to use some reclaimed methanol, because our recovered methanol always tests pretty high. It still helped, but I will only use it now as a last resort.


powering
2 bobcats, an excavator, and a ventrac mower. looking for a diesel weedeater!
 
Location: morgantown wv | Registered: June 18, 2008Reply With QuoteReport This Post
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Hey all,

This thread has been rather helpful to me over the last month or so. We are working on oil with an FFA content of ~4% which titrates between 7-9 KOH. Using some of the information in here, we have been able to get the FFA content between .94% and 2% using minimal amounts of methanol and acid. I kind of took a risk and have been using it in 1500 gallon batches with relative success.

I have a brief thought in relation to the excessive mixing causing the random rise and drop in the FFA numbers.

Would this have anything to do with the acid-catalysed transesterification reaction taking place at the same time? Albeit at a much slower rate? Is the acid breaking the triglycerides into FFA/Glycerol, causing the rise in titration values, and then dropping once those liberated FFA's are esterified to methyl esters, once again lowering the T value?

This is the only thing I can see as causing these titration fluctuations during processing.

What do you think?

Danny
 
Registered: March 08, 2011Reply With QuoteReport This Post
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not likely.
the typical rise in titration is shortly after adding the acid..

this makes sense to me..acid + FFA results in a higher titration than before adding acid. but this is short lived..the acid/methanol starts to work on the FFA lowering the titration.

varations long after the initial mixing might occur because of poor mixing before checking the titration. the acid/water/methanol will move from the oil..it might move up or down!!

-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 )
2006 Jeep Liberty CRD Smile - the wife's
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everything run B100 when its warm enough Smile
 
Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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Hi everyone...I realize I'm late to the party here but I suppose better late than never Roll Eyes

I have a question concerning the AE method. I've read the entire thread and BOY, have I learned a lot. I work for our utility system as a wastewater treatment plant operator. I've made bio using the base catalyst method with great results but the feedstock I'm using now is Ting at ~23-25 and naturally the "standard" way of processing isn't going to work. I've started using the AE method in the lab. I currently have a 2L beaker with 1L of oil in it, on a magnetic stir/hot plate. T is 23. I used a 0.17 multiplier, 20% methanol, 60% of that in the acid stage. I process at 55-60C. I mixed the methanol/acid in the oil for 2 hours and then turned off the stirrer and maintained heat. After the 2 hour mixing, I started take T at that point and every hour thereafter. (I stir the mix for 5 mins before taking T sample). At the end of the first 2 hours T droped to 15.5, the next hour, T was 13.3, next hour was 12.5. I skipped the next hour so as to give the mix a two hour span of heat without being stirred. The next hour T was 10.2, the next hour was 10. At that point it was time to go home. I had to turn the heat off because its not thermostatically controlled. My question is this...will I be ok to remix/heat tomorrow morning and expect T to continue to drop or should I drain and start acid stage again? I think the T will come down way more but I don't know if I can use the first mix by reheating/stirring or should I start a second acid stage. Thanks to everyone here for this invaluable site! Oh, this will be a touch off point, but since there is no intro thread, I'd like to share what we're doing at my utility system with bio...

We have rules, of course, for restaurants to prevent them from dumping waste oil down the drain. Private residences are a different story. Our goal is to begin a program whereby we provide our residential customers a free one gallon plastic contain to put their used oil in, let them drop it off when its full and we give them another container. Our main goal is keeping that oil/grease out of the sewer system, keep our guys on the crew from having to respond to so many blocked sewer lines due to oil/grease, reduce the fines the EPA slaps on us for those sewer overflows, and provide a great customer outreach program. Plus, we can run our backhoes, tractors, skid steers, etc on the bio. How great would it look to see your local utility's equipment out there getting the job done with a sign on it saying, "powered by X utility's customer's used cooking oil."?
 
Location: The Volunteer State | Registered: July 07, 2011Reply With QuoteReport This Post
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reheat and mix, when no further drop in T, settle drain some junk from the bottom, then repeat EA if required. so far your results are great! Don't forget,ending t will be 2 for every ml of acid/ltr of oil. so if you use 1.5 ml acid t won't drop lower than 3.


" 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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quote:
Originally posted by Biotom:
reheat and mix, when no further drop in T, settle drain some junk from the bottom, then repeat EA if required. so far your results are great! Don't forget,ending t will be 2 for every ml of acid/ltr of oil. so if you use 1.5 ml acid t won't drop lower than 3.


"ending t will be 2 for every mL of acid/ltr." Ah, missed that part. So I'm really close now. I used 4mL H2SO4, ACS grade, so 8 is as far as I'm going to get....I'm really close after 8hrs of processing where my last T was 10. Not bad....original T of 23 to a T of 10 in an 8hr process time. Of course, 1L is way different than a 151L batch!! Thanks so much for the input and guidance! As soon as I finish up my CBOD5 testing, which will free up my stir/hot plate, I'll remix and heat. I'll post back with time table for the final 2 T points to drop. Thanks again!
 
Location: The Volunteer State | Registered: July 07, 2011Reply With QuoteReport This Post



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It also looks like I could use a much lower multiplier as well. I'm assuming the multiplier is just a percentage factor for the overall T #?
 
Location: The Volunteer State | Registered: July 07, 2011Reply With QuoteReport This Post
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Got some high T oil(13) here and hope to try some AE.Will a copper cylinder be ok with this concentration of acid?
Thanks in advance
 
Location: Meath | Registered: November 26, 2007Reply With QuoteReport This Post
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