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Hi all you biodiesel nuts. Ive been messing around with this acid reaction for about a year now because my supply oil is getting worse and worse. First couple times I tried in lab it was a failure. could not figure it out. Read tons of newsgroup threads tried different things and now finally I am living in heaven.

I have a 750 gal converted steel kerosene tank as a reactor, 40kw electric heater, 2 HP pump and a 75Kva generator running off bio. All piping is black steel with brass ball valves. I process about 400-500 gals at a time.

My first successfull acid batch was last month. went from 22 KOH to a 6 KOH titration. My most recent batch, today, went from a 23 to a 1.5 (no kidding). I used the formula (titration-desired)x 0.2 for acid and used 10% by vol of MEOH. added acid to meoh very very slowly. Im doing a 500ml base rx right now to see where im at. Its hard to estimate how much MEOH is left.

Secret: Its all about the water.

I got tired of filtering and drying so I found a 1000gal fertilizer tank and turned it in to a settling/storage tank. All the oil I collect goes into it and settles for a week or more. That way all the garbage and water settle to bottom and I use the top portion. I also add a gallon of 50% NaOH to the tank when filling. I get nice clear oil when I need. Yea I know im gonna have to empty it one day, yukkk.

First thing I do is heat the oil to 220F for an hour or so, let it settle overnight drain the water and proceed to the acid Rx.
After acid Rx I let settle overnight and drain 30-40 gals of black watery liquid, then do another acid Rx using 5% more MEOH and (titration-desired)x 0.1 for acid. Let settle over night and drain about 20 more gals of black liquid.

Mix up, take a 500 ml sample and do a lab size base rx to figure out how much MEOH I will need. I probably use to much meoh but my cost is still less than 1.25$/gal finished.

I am sure there are ways to improve and optimize but right now I am happy to be able to use this crappy oil. Thanks to all who have helped me with this method. Ive left out a lot of details but basically its like every one who has had success.


02 duramax, bio since 04/08
 
Location: St Pete Florida | Registered: December 29, 2007Reply With QuoteReport This Post
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hootep
-using your Rx I would need 288ml of acid to treat 160 ltr of T 10 wvo with a target T of 1, or did I miss something. Right now, I use .65ml of acid per ltr or 104 ml of acid for the batch.
-if you are adding caustic to you wvo holding tank, how do you get an accurate T to start? is the caustic not turning some ffa to soap?
-the other part I don't under stand is the need to base process a 500ml sample to see how much caustic you will need, all you need at this point is a simple T test after the finnal ae, just be sure to mix the batch well prior to T sample.
-you have to remember also, the more acid you use for ae, the more water that will be created in the following base process when the acid is neutralized by the caustic. 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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Hootep,
welcome to ACID side of BD making.

I think if you check you oil..even after you think you have it dry.its not..

does your oil pass the HPT test..you did check this right?.. this is just start of dry enough. but a long way from dry.

I would suggest not adding the 50% NaOH to the oil before processing..why you might ask..
well soap? oil/water/caustic makes soap...why convert your oil into soap? but its your call.

why guess on the base reactions? these are known..well known..you use the other 10% or so.


why add the acid/methanol slowly? why mix the acid and methanol before adding to the oil?
take some time and read the sticky thread at the top of the forum..yes you'll learn 100x more about acid processing than you know at the moment..trust me..Smile

-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
99 dodge 2500 5.9l 24v..-mine Smile
everything run B100 when its warm enough Smile
 
Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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BioTom,

you beat to the some of the punches..
but I agree with you..of course SmileSmile

-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
99 dodge 2500 5.9l 24v..-mine Smile
everything run B100 when its warm enough Smile
 
Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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quote:
-using your Rx I would need 288ml of acid to treat 160 ltr of T 10 wvo with a target T of 1, or did I miss something. Right now, I use .65ml of acid per ltr or 104 ml of acid for the batch.


Im just using the formula thats been described here often. So maybe I can get a way with less but right now I dont. 0.22$/lb 98% sulfuric is no biggy. It works!!!


if you are adding caustic to you wvo holding tank, how do you get an accurate T to start? is the caustic not turning some ffa to soap?.[/quote]

fatty acid insoluble in water, fatty acid salt= soluble in water, remember settling tank has water in bottom NaOH and salts settle out in water phase.


Because I dont know how much MEOH is in the reactor. I drain bottom after acid process till blackness goes away which is usually 50-70% of acid rx meoh added.


-you have to remember also, the more acid you use for ae, the more water that will be created in the following base process when the acid is neutralized by the caustic.


I will assume that with a titration of 2 KOH I have drained all the acid out. You create water with the creation of fatty acid salts, and the esterification too. And the black discharge contains alot of water loving MEOH.

Hope this comes out right visually with the quoates and all.


02 duramax, bio since 04/08
 
Location: St Pete Florida | Registered: December 29, 2007Reply With QuoteReport This Post
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quote:
Posted 06 January 2010 06:56 PM Hide Post
Hootep,
welcome to ACID side of BD making.

I think if you check you oil..even after you think you have it dry.its not..

does your oil pass the HPT test..you did check this right?.. this is just start of dry enough. but a long way from dry.



I agree its not dry but thats why I have to do a second AE. Thats why I have to use the extra meoh. The first ae does a good job of getting rid of the residual water.

I think the next time I do this I will use only 7% of meoh and 0.1 factor for acid on first AE and same for 2nd AE. I believe that 1st AE does a good job of scavenging the water which is why the 2nd AE does so good. 1st AE generally goes from a 23 KOH to a 16 KOH and 2nd AE gets it down to less than 4 KOH atleast on my most recent batch.


02 duramax, bio since 04/08
 
Location: St Pete Florida | Registered: December 29, 2007Reply With QuoteReport This Post



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if you dry your oil more..you'll find that the first AE will drop more..think 5-8KOH instead of 16.

true FFA are not water soluble but NaOH/FFA/water makes soap...you're loosing oil..that could be converted into BD. not to mention the if any NaOH says around in the oil as emulsified water..as soon as the acid mixes with the oil you're creating WATER..just what you don't want.

as for how much methanol is left after draining? how much did you start with? how much did you drain..yes about 90% or more of what you're draining is methanol. its a mix of methanol/acid and water. I hope you have a methanol recovery setup..

if you know how many mls of acid you're using per liter..multiply this by 2.2..this will tell you how much the acid raised the titration. yes raised..if you convert 100% of the FFA to BD then you have a 0 titration.

-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
99 dodge 2500 5.9l 24v..-mine Smile
everything run B100 when its warm enough Smile
 
Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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Hoot
-water kills the AE process, with T 23, the water created in the ae process coupled with the starting water is the main reason 2 ae processes are required. I don't know of anyone who can treat T23 wvo in one step.
-The calculation that has been around for several years is for sure outdated. having said that, if your wvo is not very dry, HPT minimum, then for sure more acid is required. depending on the molar weight, the methanol acid can either float or sink, so I would ,if I could , do the calculations to see if in fact i was draining the methanol/acid phase. Double d and D Kenny are the resident experts in this area IMO.
-after I drain 5 ltrs of methanol acid crud,I mix, do t and I add this 5ltr of fresh methanol to the base stage. no requirement to further test anything.
-I applaud you in your efforts to use wvo that would otherwise produce very poor yieds, and also ecourage you to read the lastest up dates on this process as DKenny suggested above. I also agree many people are missing out!!!! 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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Dave
-why arn't you at work Big Grin Big Grin


" 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 Hootep:

if you are adding caustic to you wvo holding tank, how do you get an accurate T to start? is the caustic not turning some ffa to soap?.
quote:
fatty acid insoluble in water, fatty acid salt= soluble in water, remember settling tank has water in bottom NaOH and salts settle out in water phase.


The salt/soap is soluble in both oil and water. One end is hydrophobic and the other end is hydrophylic. I would expect the highest concentration of soap to be closest to the water/oil interface.

quote:
Because I dont know how much MEOH is in the reactor. I drain bottom after acid process till blackness goes away which is usually 50-70% of acid rx meoh added.

Draining the water layer completey is a good thing if your going to run a second acid stage. Otherwise your going to start the second round at a disadvantage. If you can get the titration to drop enough after the first round you may not need to drain after the second round. You'll start the base stage with more water in it, reducing yield a bit but your savings in methanol may be worth it. It's a personal preference thing.

quote:
I will assume that with a titration of 2 KOH I have drained all the acid out.

Or you've esterified almost all the FFA and your titration is reading sulfuric?

quote:
You create water with the creation of fatty acid salts, and the esterification too. And the black discharge contains alot of water loving MEOH.

Agreed Smile

Congrats on the success. This process does seem to give some folks a challenge.


Hope this comes out right visually with the quoates and all.[/QUOTE]

This message has been edited. Last edited by: Double D,
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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quote:
why add the acid/methanol slowly? why mix the acid and methanol before adding to the oil?

What your saying is you can add the acid and methanol separately to the wvo? NO way I lost two batches that way,this past summer. On the third batch I added the acid to the methanol slowly ,because you can hear the methanol react and that batch worked. Do you add your lye or KOH separately and then the methanol ?or the other way around methanol first and then the caustic when you do the base reaction ?either way it doesn't work .
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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heat
-how long have I been doing the ae process?, I never mix the acid and methanol togeather first!! I add methanol, hold back 2 ltr, mix well, add the acid, then use the remaining 2 ltr to flush the acid from the ball valve, then mix and let sit. Not sure what your problem was, but can we say water Big Grin 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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biotom,

you of all should know its too COLD..besides I've been woodworking..inside work not outside Smile
ok not as COLD as where you are..but here in NC its COLD!! when you have to work outside and is 95F in the shade..remember this..that my normal day in the summer not just a heat wave..Smile so think 3-4 months of the year not just a week.


as for adding stuff together..
for the record..
when I started out using AE..my that was a long time ago..it was normal/common to add the acid to the methanol first..so this is what I did..and it works..

well others joined the AE world..
some added the acid to the oil first..
well sure enough I have to verify their ideas..I needed them to verify mine?
guess what..it also works..no difference..hum??? heatbeater I would suggest your failures were do to something else..not how things were mixed nor when..

adding rate.. another topic for debate..
yes I have run a large range here..
20+ minutes to add 7 gallons.my normal batches are around 60 gallons of oil..to well how long does it take to pour out the mix from a 15 gallon drum..10 seconds..20 seconds?? difference..no!
the AE process is a slow process..unless it HOT!..also doesn't make a difference during the base stages either..

now for some tougher questions??
pumping rate? turns per minute?
other methods?
how its all mixed makes a bigger difference than how long to add the ingredients..
but many find just mixing until mixed is enough for AE.
during the base stages the better/harsher mixing is WAY better! no question. no doubt.

time for dinner..
-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
99 dodge 2500 5.9l 24v..-mine Smile
everything run B100 when its warm enough Smile
 
Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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heatbeater
-I believe your situation resulted from a combination of wet wvo and residual caustic contamination in the processor since you do both AE and base in the same tank.

Dave
- this winter has been a breeze compared to the last two. But a wind chill of -48 is too cold for outside anything!!!! 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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[QUOTE]Originally posted by Biotom:
heatbeater
-I believe your situation resulted from a combination of wet wvo and residual caustic contamination in the processor since you do both AE and base in the same tank.

Dave
- this winter has been a breeze compared to the last two. But a wind chill of -48 is too cold for outside anything!!!!
-ae first came out at JTF, and the process was to add the chemicals one at a time!!! 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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Biotom,

if you reffering to the 'foolproof' method..just check the success rate..not so go..so you can understand my reaction to anything from JTF.. please try not to laugh too hard..

I would also be skeptical that JTF had AE first.. you'd have to check the archives here but I do remeber reading posts from '01 on AE..I read everything I could find before I first tried AE..long before I wrote 'my method'..

either way I really don't care who was first..I just know WE have perfected the method far beyond JTF, FATTA, and ISU methods..

-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
99 dodge 2500 5.9l 24v..-mine Smile
everything run B100 when its warm enough Smile
 
Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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quote:
how long have I been doing the ae process

The wvo that I AE'd titrated 15. i haven't made any bio since that 3rd batch. Does your's titrate as high? I was afraid to mix the 2 together but finally give it a try . I can't see how the chemical reaction can work by putting them in separately,but I'm not a chemist. What do you do for the water test /anything other than the HPT? I'd like to buy the test kit . I need someplace where its heated so I can do some brewing ( I said heated ,not on fire)HA HA. I have some spare time right now ,but when the weather warms up it'll be a different story. The only thing I can say about my dewatering ,is I heat the batch to 140 F and circulate maybe every 6 hours,sometimes for 2 days until a HPT shows no condensation on the glass lid. I did a HPT once on some fresh wvo and it blow the lid 5 ft into the air, good thing I wasn't standing there at the time.Lesson learned HEAT SLOWLY . I wouldn't want that to happen with 40 gallons of wvo.When I dewater there's usually a gallon or two of gray goo that settles down and I drain off before I recirculate. I wouldn't think a film of bio from the last batch would leave enough KOH to hinder the AE?
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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quote:
Originally posted by Biotom:
Hoot
-water kills the AE process, with T 23, the water created in the ae process coupled with the starting water is the main reason 2 ae processes are required. I don't know of anyone who can treat T23 wvo in one step.

What do you mean you dont know anyone that can do 23T oil in a single stage?!?!? :P
I gotta start posting more Big Grin
 
Location: Buckeye | Registered: July 07, 2009Reply With QuoteReport This Post



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Has anyone tried using Zinc acetate as a catalyst, it is supposed to do both acid and base in the one reaction.
 
Location: Nimbin Australia | Registered: December 04, 2007Reply With QuoteReport This Post
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hootep, heatbeater,

wrong crowd if you think T23 is 'bad'..

sorry but T23 isn't even close..think 2x or 3x of this number..yep..I ran several batches..not a test sample for T46 oil last summer..and that's not my highest titrating oil..as bad as my oil is..I know I don't have a lock on the worst that would fall to buckeye or akwrench..If I recall their's is normally 3x your T23...so be glad you only have T23..fyi..If I could have all the oil i needed but to titrated at 20+..I'd take it Smile

for water testing..
after its passed the HPT..by the way..heat a plate until its HOT..drop 0.5ml or so on to the plate..what happens? anything other then smoke..too much water.. you should not see bubbles in the oil..ZERO!!NADA..any bubble is a FAIL!..but its not dry yet..my last couple of batches I bubbled air in the hot oil with the vent open on my reactor I watched for steam..place a cold glass plate near the output..any condensate? oil isn't dry..keep drying..YES that dry..

-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
99 dodge 2500 5.9l 24v..-mine Smile
everything run B100 when its warm enough Smile
 
Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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