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HELP!! ~200 gallons of oil titrate ~ 25 NaOH
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I am about 14 pages into the super long 80 page thread. So far I have gathered the following:

1) I need to be sure my oil is super dry to start with
2) I will likely need to 2 or more Acid stages, and drain in between.

I just got my sulfuric acid yesterday. I plan to do 70 (WVO) batches.

For the "long thread" I have seen clues that there may be advantages to using different amounts of acid and methanol for higher tirating batches. I guess I am "pussing out" and asking if anyone has any advice on what formula(s) I should use.

Please help me!

Should I just go with (25-3)*0.18 (ml per liter of oil (which for a 70 gallon batch would be 1050 ml of acid) and 12% methanol (8.4 gallons)?

Or are different amounts/formula appripraite for the first acid stage when oil titrates at ~25 (I need to get a batch size together, ensure it is dry and then perform a final "for the run" titration). I have 4 liters of sulfuric acid, a fresh drum of methanol and 200+ gallons of bad WVO.

I have read that mixing left on a long time does not help (and may hurt). I have read to drain about half the qty of methanol after the first AE run, mix it up and then tirate to get the interim results. (And to add that amount drained to the remaining (10%) methanol for the base stage.


Any advice is apprecited and thanks in advance!


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Registered: March 13, 2005Reply With QuoteReport This Post
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You can break it into 2 stages if you want, but here's what I would do on a single stage reaction. (I recommend testing in the lab first.)

The following is the recommended procedure that my BIB 2.7 software recommends as a starting point for a single stage reaction. I assumed it was a 100 gallon batch to make your work easier. That way the methanol and catalyst volumes are per 100 gallons of oil.

I'm a little leary of using this much catalyst, but my program is design to keep the "reaction time" about the same for all oils so it boosts up the catalyst.

If you try this, let me know how it turns out. The people that use my program generally don't have oil that titrates higher than 20 so I don't have much data in the 20-30 AV range. Also, please try and find out how much water is in your oil so that the results have context.

Date
Time
Description

Oil Volume 100 gallons
Oil Molar Mass 847 g/mol <---
Oil Density 0.910 g/cc
Acid Value (from titration) 25.00 mg KOH/g Oil
Calculated FFA 12.58%


Recommended Reaction Mixture


Oil of Fat Feedstock 100 gallons
Methanol 27.9 gallons
Sulfuric Acid 0.34 gallons
1272.14 mL
2328.01 grams
5.13 pounds
 
Location: CO, CA, KS, or FL | Registered: January 17, 2009Reply With QuoteReport This Post
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Marky
-that formula will work but IMO it uses too much acid and too much methanol. If I were processing this wvo I would use this formula, T * .095 * ltrs of wvo: then use 10% methanol instead of 12.
-if you mix the batch continuously the ending T will be higher, this is more likely because all the acid is in the mix, it doesn't get a chance to settle out.
-Dry wvo is a must, and the higher the titration the more water the oil can hold.
-The higher the heat the faster the AE process. If you can hold the heat at 165f and mix continuously to keep the methanol mixed in the process could be done in a couple hours, otherwise maintain 130 f and let stand overnight. check T
-Drain an amount equal to 1/2 of the methanol used in this stage, then add methanol and acid repeating the steps used in the first AE stage. ( methanol + to the amount of liquid drained)use T*.095 * TOTAL ltrs in the tank to determine acid amount for second AE stage
-hope this helps 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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-Another point to concider when determining how much acid to use is the caustic load that remains in the processor after the batch of biodiesel is removed, it takes very little caustic to neutralize the acid to a point where AE fails to esterfy the ffa. I try to keep the acid amount to an absolute minimun to reduce the amount of water created when the acid is neutralized by the caustic in the base stage.
-The two main reasons people have poor results with AE are wet wvo and caustic contamination.
-Not sure how much experience you have so I'll just say be careful with the sufuric acid, have running water at hand and a box or two of baking soda along with the normal personal protective stuff required for safe base processing. 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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it also helps if the oil is clean.
the in long thread, Buckeye started with worst oil, but it was clean and dry. He also used far less acid than what biotom is suggesting. interesting that helpinghands acid qty is almost then same as T*0.95 if T is in KOH.

it works like this
wet oil - more acid -> higher ending titration compared to clean dry oil not the starting titration
dirty oil - more acid -> might have a higher ending titration
wet oil - more methanol -> lower ending titration if the acid qty is kept down
dirty oil - more methanol -> lower ending titration if acid qty is kept down.

unless something in the processor or the oil consumes the acid it will remain.
25 NaOH is equalivant to 25*1.4 = 35KOH..high but usable..without a question.

here's an example
35 * 0.1 = 3.5ml/liter of acid
3.5 * 2.2 = 7.7 for a titration caused by the acid using KOH or 7.7/1.4= 5.5NaOH
the 5.5/7.7 would be the best titration you'll see using 3.5ml of acid

I wouldn't use 27 gallons of methanol for a 100 gallons of oil..WAY TOO much for a single acid stage. that's 27%..then you need to add the methanol for the base stage(s)

you might need 25%-27%(total) for 2 stages of acid and base stages.

if you have any doubt on the amount of acid to use..use less then you think you need.

-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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If you are removing and reusing a portion of your acid/methanol leyer then you don't end up actually using that much methanol and oil.

How much methanol and acid you need to use is dependent on what your "target" acid value is.

Compare the different methods presented by various people here in the lab and see what acid values you end up with.
 
Location: CO, CA, KS, or FL | Registered: January 17, 2009Reply With QuoteReport This Post



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My processor is an old modified well pressure tank. It has a "kinda half sphere" on the bottom. Kind of like an air compressor tank I guess. (It is about 92 or so total gallon capacity). I know I cannot process an 80 gallon batch with 20% methanol anyway). It drains out pretty well, but it is not perfect.

I was thinking I should wash the processor out first with a load of water and some HCl or vinegar. Couldn't hurt I think (with the possible exception of leaving some water behind.

Guess the only thing to do is give it a go, and see what happens. I have a good pump on it and I think it pumps 20-25 gpm (not ideal, but better than a HF pump by a long ways). I have the return going into the top of the tank (it splits into two before entering the tank and the pipes are complimentary angled where they are welded on so that the whole mix will turn. I think it blasts and turns the mix pretty good, but of course I cannot see it. In any case, there should be no methanol floating on top.

(Helping Hand - I am a little "taken aback" by your suggestion to use 27 gallons of methanol for the first acid stage for a 70 gallon batch. You did mention that you calculator was mostly used by people with much lower titrating oil though, I wonder if my high titrating oil skewed the calculation.

In any case, I will study the help already given above and pick my numbers and give it a try. I'll let you knoiw what happens.

Thanks

Thanks for the help so far.


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Registered: March 13, 2005Reply With QuoteReport This Post
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Marky,

do you have a vent on the top of our processor? it would great if you did..

can you inject air while the pump and heat are running..
if so I would suggest
loading the oil
add heat
mix and pump air while holding a temp around 150-160F
if you can take a cold glass and hold it in front of the vent without condensation forming. then your oil is dry.

helpinghand,
using that much methanol during the acid stage will cause another problem. the water/acid/methanol mix will float on top of the oil. making it next impossible to drain out. using less methanol 10-12% will force the mix to sink. I'm sure you are aware that to reuse the drain mix the methanol must first be distilled. or processed to remove the water.

-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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Yes I do have a vent on top.

I can also inject air "near" the bottom while the pump is running and heaters heating.

(I am assuming it is best to have the pump running and blow the air through the oil). I must admit one of my apprehensions to this AE thing is the potential need to hold the heat overnight without mixing. I may insulate beter before starting this. I should anyway.)

Hopefully I wil be getting to it this weekend

Thx

Marky


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Registered: March 13, 2005Reply With QuoteReport This Post
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if you can heat without pump it doesn't matter. heat and air will dry the oil. Are you concerned about the overall energy consumption?

With my setup I cannot heat with the pump running. My element is inline with the plumbing.

Insulation is always good.

please keep us informed...

just know there are several of us who have been done this road first.

something else you might have happen..if your pump is big enough just circulating the oil will get it hot. Mine does..its slow but I don't need to add electric heat. just a thought

-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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Marky,

Dont know your knowledge of biodiesel, but I will say this- Listen to Dave and Tom. Dave converted me over to AE about this time last year. Our plant runs our fleet of trucks(60+) on B100 daily. When it comes to the AE process the information Dave has given me is invalueable. Tom's math figures when it comes to AE are right on target time after time. Use to worry about every 6000 gallon load of WVO we brought in. Now I just request that it be dewatered as much as possible so I dont spend all my time drying it. Once its dry the FFA content doesnt bother me at all. Use their figures to a exact specifications. Dry the stuff more than you can imagine. Once dry dry it again. We now run 2500 gallon batches of WVO in AE. We then move it to 1000 gallon processors. My biggest problem was putting the acid in the oil before the methanol. Dont get me wrong it is not any sort of problem unless you are partially color blind it does turn the oil a darker tint so harder for me to see the seperation. Read all 70+ pages of the long thread, but pay attention to Dave and Tom. I am proof their process works daily on large batches. Tom is right about heat. Just put new heaters in one of my holding tanks where i can get 3000 gallons of oil upto 165+F in 6 hours. Ran batch today where titration dropped from 12 to 3.9 in 1 hour at 155F heat. Heat was reason IMO. Ending titration was 2.25 in less than 3 hours. It works Marky. Listen to them.

Dave-Come visit again will give you some more cheap methanol. We are less than 4 weeks away from completely solar at our facility in all 3 buildings then will sell the excess electricity to local power company. You would like it.

C
 
Registered: August 26, 2009Reply With QuoteReport This Post
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Sorry for the no updates.... I was going to knock out a batch of normal oil first (figure this AE might be tying up my processor for a "whiles"), I was heating/pumping/filling my processor, and I heard the pump quit pumping. The motor was still running but...(I heard it happen, i was sittng right next to it. Turns out the bottom plumbing was completely plugged. I have been demthing in the processor (WBD), and yes, I did let a couple of half batches of demethed bio sit in it. Plugged solid with that gojo/goos type soap. In any case, I had to take the pump cover off and all that, and am using this opportunity to clean the processor slimy outside, do a lot better job of insulating, have a fitting/weld on the top that broke loose some, and stuff like that. Had a heck of a time getting the oil load out. I think a big chunk of that soap broke loose (and it was already pretty plugged/blocked. I thoight I lost my pump (Teel/Daytom, nice one I think)I figure a very well insulated processor is going to help this whole AE thing, drying oil, holding heat, etc...... Thing is....."I ain't as good as I once was" (takes me a while to do this kind of stuff).


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Registered: March 13, 2005Reply With QuoteReport This Post



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WELL??
any news?

-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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Welll not exatly the news you want to hear (I am guessing)m but I just took the final on my class tonight (and passed with a good score). It was weekdays 2.5 hrs per day and REALLY put a cramp on my biodiesel brewing. But my processor repaired and is "almost" got a full "coating" of sleeping bag/camping mat. Gonna insulate some more and put it back together and get it into operations SOON. (I promise).

Gonna insulate the top more for de-watering/de-mething.

But no news on the AE of the oil yet... sorry


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Registered: March 13, 2005Reply With QuoteReport This Post
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OK giuys.. I am heating (for de-watering first) some 75 gallons. I just titrated it at 19 NaOH (I was pleased, considerably better than the 25-30 I was expecting).

So 284 liters, T=19; 19 * 0.095 * 284 = 512ml of acid. 10% methanol = 7.5 gallons. I will note the time I add the acid (first) and then the methanol, pull the methanol into the mix over 10 minutes, mix another 10 and shut it down.

One problen (not fixed yet is my thermometer is broken). So, I guess I am going to "guesstimate temperatures through this batch.


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Registered: March 13, 2005Reply With QuoteReport This Post
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Marky
-if you add the methanol first then mix for 5 or ten minutes then add the acid and mix, the resulting biodiesel will be much lighter in colour. 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 will do that Tom.

I did not get past dewatering yesterday.....I got the temp up to (per a meat thermometer dipped into a gatorade bottle) 210F, blew air and out the top for several hours, them turned the heat and pump off, switch the pump so suck air from the bottom and out the top for a few more hours. I switched back to blowing air in the bottom (to use the cold glass of water test), and it looks like the water is pretty well out. Temp was down to about 190 by the time I went to bed. Hopefully it will be cool enough to process when I get off work. I guess I will just be slowly adding the acid in through the top (after sucking in the methanol) thru a funnel.


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Registered: March 13, 2005Reply With QuoteReport This Post
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I got gutsy and put on my "gear (full face shield, gauntlet chemical gloves , old jacket, hat, etc.) and added the acid to the methanol real slow. I didn't have any bad incidents, BUT... I took probably several minutes to pur in a half liter of acid to 7 gallons of methanol. It seems from hearing tha banging and such when the trickle of acid hit the methanol, that had I just dumped it in, it would have been extremely violent. I had a funnel with a big hole so as not to "airlock" . It was duct taped to the big bung on my carboy with some air allowed to pass. Anyway.... that was pretty exciting

I sucked in (temp at 135 F) the acid/methanol over a 15 or so minute period, ran it another 15 without heat, turned the heat on, ran it another 30 minutes and shut it all down (7:30 PM)

8:30 PM titration was ~10.5 (I am pulling samples for titrations from very low on the tank, probably 10 gallons or so from the bottom - not sure if this matter, but I am guessing low in the tank will titrate higher than high in the tank)

10PMish - titration about 8.5. Then I turned the heat on (no mixing though) for about 30 minutes (top vent open with ~4 foot copper reflux pipe). Then closed the top valve for overnight Hopefully I did not loose to much methanol, but I ws trying to get it/keep it good and hot to help the process continue as it set overnight.

I did pull a sample and watched it for an hour or so, and saw no signs of anything settling to the bottom, and the oil was clear before adding the acid/methanol, but the sample is/was pretty cloudly looking.

Thats all I have for now - so far so good I think - will know much more when I get off work.
I will drain mix and titrate this evening after work. What do you think it will be?


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Registered: March 13, 2005Reply With QuoteReport This Post



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Marky
-sounds good! let the process run until there is no more drop in T. A sample taken from near the bottom will have a higher T valuue than one taken at the top as the concentration of acid will be greater at the bottom. once the process is finnished, drain, about 1/2 the volume of methanol used, the crud from the bottom,then mix well and check your titration. I expect that given the amount of acid you use your lowest T will be about 4.
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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Starting T = 19, 75 gallons of oil, 7.5 gallons methanol + 512(ish) ml of methanol and 22 hours later the titration (bottom sample again, not yet drained or stirred) is 5.4. Temp is about 110F right now. I can;t remeber what temp that AE stalls, but seems like I read about 120F?

I am thinking - heck ya...!

Wondering what I should do....options i see....
1) nothing for another day
2) turn heat on and heat it back up without pumping/mixing (I know this will mix some though)
3) drain 3.75 gallons and and heat it back up without pumping/mixing).
4) drain 3.75 gallons, add 0.095 * 5.4 * 78.75 gallons * 3.785 gallons per liter = 152 ml of acid and 3.75 gallons of methanol heat back up and do another AE...

Any opinions?

Guess I could also proceed to base process/finish too!


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Registered: March 13, 2005Reply With QuoteReport This Post
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