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Last night went I left, T was at 10. This morning I remixed and heated. Mixed until the mixture came up to 60C and then shut off the mixing portion and continued heating. After one hour of additional heating, T dropped to 9.5. I allowed the mixture to continue heating for another 2 hours and T remained at 9.5. So, I've shut down the acid stage. I'm going to allow it to sit and settle all weekend and run base stage Monday morning. I'm sure I could have got T down the additional 1.5 but I'm anxious to proceed. Beginning T= 23. Final T= 9.5. Its like getting a new lease on life!!

One correction...original T was actually 26. 26-3=23(0.17)=3.91 (I rounded to 4mL)I believe I'll try a lower multiplier next time, maybe 0.16 or 0.15. Thanks again!
 
Location: The Volunteer State | Registered: July 07, 2011Reply With QuoteReport This Post
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Copper will work steel also works.


" 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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Acid amount I find the dryness of the oil and T will dictate how much. for t20 1.7 - 2 ml will work if the oil is dry. t8 - 12 can be processed with .75 ml/ltr with dry oil. If getting the oil dry is a problem like it was here last summer just up the acid amount. I have been using 3ml/ltr with t 16 18 NaOH oil with great results. the only drying the oil gets is to stand in a heated tank 140f for two days then into the processor.


" 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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Not sure how your processor is set up. But if you can drain and are not using high temp AE you could also consider not mixing during AE.

We mix while methanol and acid are being added and then actually turn the mixer off and let is settle overnight. After draining the 'acid drainage' and remixing, typical results are 34->4-6 and 20->2-4 using this method. Never actually compared how this worked to HTAE but ours can sometimes take over 24 hours to react depending on how high the initial water is and the higher the final acid # will be.
 
Registered: February 25, 2010Reply With QuoteReport This Post
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My latest oil has jumped to a "T" of 18 koh and am considering AE so----

I need some help understanding--

Below quotes from BioTom seem to be in conflict-- If I use 3ml/ltr of oil what can I expect my ending "T" to be ? 6 or 1.5 ?

Tnx,

ReM



"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. Tom"



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.


B100--
2004 Motorhome CatC7
1987 Mercedes 190D 2.5 Turbo(possibly for sale)
1983 VW Pick-up (Caddy) 1.6 Turbo
Southern Oregon
 
Registered: May 23, 2004Reply With QuoteReport This Post
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I'm still using Kennys original formula with great success, starting T-3x.20=ml/L of acid.
I still add acid and 30% of the methanol and heat and circulate continuously, my T will drop within 2 hours to it's lowest point, at that point I do a titration and a regular single base process, works every time.
 
Location: West Michigan | Registered: April 26, 2006Reply With QuoteReport This Post



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quote:
Originally posted by fabricator:
I'm still using Kennys original formula with great success, starting T-3x.20=ml/L of acid.
I still add acid and 30% of the methanol and heat and circulate continuously, my T will drop within 2 hours to it's lowest point, at that point I do a titration and a regular single base process, works every time.


Thanks for the quick response--

Can you please clarify you methanol % ?

Kenny uses 60% for the acid stage and you are saying you use 30% ?? Correct?

ReM


B100--
2004 Motorhome CatC7
1987 Mercedes 190D 2.5 Turbo(possibly for sale)
1983 VW Pick-up (Caddy) 1.6 Turbo
Southern Oregon
 
Registered: May 23, 2004Reply With QuoteReport This Post
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I make 350 gallon batches and I use 22% methanol so the entire batch takes 75 gallons, for the acid stage I use 35 gallons, so that's like 40 something percent, I really don't think the exact percent is that critical.
 
Location: West Michigan | Registered: April 26, 2006Reply With QuoteReport This Post
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quote:
really don't think the exact percent is that critical.

I shoot for about half of the total methanol I will use, but really you only need to use enough methanol that the acid will add to it without increasing its temp to boiling. You want the methanol: acid ratio to be SAFELY methanol heavy, by a factor of 10,000, at least, I'd say.
 
Location: Southern WI, USA | Registered: May 18, 2006Reply With QuoteReport This Post
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I'v had unsatisfactory results on the first acid step before so I've put 300ml of acid in 5 gallons of methanol and injected it into 350 gallons of oil and it did the trick, it just shows how little will affect so much.
 
Location: West Michigan | Registered: April 26, 2006Reply With QuoteReport This Post
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ReM by allowing the acid to settle to the bottom then draining the junk you can lower the ending T beyond the 2 * ml of acid you get if you don't settle and drain.


" 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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Hello you lovely folks in the USA I asked a few questions because I hadn't done any acid method in a couple of years because my oil was good but is now not as good at 7.5 KOH. I feel I've found the problem to my last batch at this titration where I didn't leave the acid stage long enough because this batch (175 lt) I'm doing now has been in the processor 6 hours and has dropped 2.5 points but it did not move at all for two hours and I was in a quandary as to why this was. I see a few of the experts get the titration to finish in two hours and wondered why this was not so with my batch. I always process at 40 C. My question is, is it possible (as per previous posts) to leave the acid process working for too long ???? I see DAVE K's oil is about the same quality as mine 7.5 KOH so I wonder what is the exact amount of H2so4 he adds to his dry oil ?
I added 210 ml to 175 Lt oil then 10 lLrs meth -- I'm looking forward to it dropping more but it would be nice to know what it might drop to.....
Kind regards Mick in the UK
 
Location: Nottingham in England | Registered: August 01, 2008Reply With QuoteReport This Post



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Fabricator ---I see you do big batches but I've got a 175 L batch going at the mo and it's taken eight and a half hours to get from 7.5 to 4 KOH at 40deg C and I wonder why this is ? I've got it circulating as well. I'm not unduly worried about it because it's going the right way (I hope) but can it be left too long without the last base stage being done ?
 
Location: Nottingham in England | Registered: August 01, 2008Reply With QuoteReport This Post
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at 65c the AE will finnish in a couple hours, at 40c it will take 12 -14 hrs.


" 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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Yes it can be left to long, the T will actually start to go back up, but you can add more acid and methanol and it will go back down, at 3.5-3 I'd keep a close eye on it.
 
Location: West Michigan | Registered: April 26, 2006Reply With QuoteReport This Post
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Thanks for the replies --- I made a stupid mistake re the temp - its's 60 C -140F with the temp gauge
2 thirds the way up in the processor... I checked it this morning & the T is 3 , so it seems to be stopped. I'll let it settle & see if there is anything to drain off ?
I wonder if my temp has always been on the high side in any case ?
 
Location: Nottingham in England | Registered: August 01, 2008Reply With QuoteReport This Post
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Another thought --- Regarding titration especially with my oil being 7.5 KOH start. If I titrate one and half hours after start of acid process should I see the respective T result of the reaction.
I think it's accepted the acid has a greater specific gravity than water so must sink in the processor but what I'm perplexed about is that I saw no movement whatsoever at one and half hours after infusing the Acid and Meth.
A long time ago Dave said I may have water in the oil but I've never seen any water ever apart from water formed after the acid reaction & then only very very little.
Biotom I think I saw somewhere stated that the acid is still there in the mixture but I wonder how much and wonder also due to the mixture being acid is this the factor that is affecting the T result?

Fabricator- Thanks re the good advice re I can add more acid & Meth........ I sure am keeping a very close eye on it... I calculated that theoretically when I left it the T should have got to T.5 after another 9 hours but no it was 3 ? I was not too worried when the reaction seemed to be going in the right direction as regards the T results so I wonder if I should drain a bit of fluid off & scrutinize it. I could even check it for PH if this would be at all informative ????? If only I could get my hands on more 2.5 oil & sack the chip shop ! !
 
Location: Nottingham in England | Registered: August 01, 2008Reply With QuoteReport This Post
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If you have it down to 3, run the base stage, there is no reason to drain anything with oil that has an initial T of 7.5.
You can battle for two or three days to try to get the T down a point and a half and save half a pound of KOH in the base process, or you can make fuel, when I get to numbers like 3 I make fuel.
 
Location: West Michigan | Registered: April 26, 2006Reply With QuoteReport This Post



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T can fluctuate during the AE process, Starting T 7.5, if you use 1ml acid per ltr then add 2 now T should be 9.5. once the process is finished, T should be about 2 if all ffa are converted. Then if you allow the batch to settle you can drain off some of the acid from the bottom and end up with T in the range of .5 - .75. Letting the acid/methanol mix sit in the oil for long periods of time will have NO detrimental effects on the AE process. I’ve tested this for 10 days no heat, results no reaction but methanol/acid floats on top, then add heat mix well and within 12 – 14 hrs AE is complete dark acid oil in at the bottom ready for draining, leaving the sample sit submerged in the heated wvo tank for a further 20 days had no affect. I use 10% methanol or less, the process works well with as little as 8% BUT the oil must be DRY. The more methanol you use the greater chance that the junk will float on top rather than sink to the bottom.
Remember, without draining after AE your minimum T will be 2 for each ml of acid used/ ltr of oil.
It’s difficult to say how much acid remains in the oil, but if you start with T 7.5 then add 1ml/ltr of acid resulting T would be about 9.5, if after 12 – 14 hrs of process time you mix the batch well and check T it should be very close to the acid amount that was added. This would indicate that the ffa is converted, then if you settle and drain, remix and titrate you will know the T value of the remaining acid.


" 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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Fabricator & Biotom Thanks for the advice of which I'm very grateful -I'll print this info off so I can refer to it as long as I live.......... I'm a bit of a wimp I feel because at about 4pm I went for the base stage KOH and put in 1.6kg +15 lts Meth & then will check as usual, re base base..... Thanks again best regards Mick
 
Location: Nottingham in England | Registered: August 01, 2008Reply With QuoteReport This Post
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