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36t and no change after AE
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Not sure whats going on here, I've done 4 batches before and they turned out beautiful.
This round the titration was really high, 36. (I use KOH).

Heated up the oil to 140 F.
Mixed 5 gallons of methanol with 750ml of 98% acid for 30 mins.
Added the mixture to the oil and let recirculate for 8 hours (overnight) at 140 f.
tested and got 36t...
I drained maybe 1 quart of black stuff with no visible water.

Where am I going wrong ? Does the treated oil need to sit/cool for a certain amount of time ?

I went ahead and added 3 more gallons of methanol with another 100ml of acid, and it didnt budge.
still at 36t.

What am I missing ?

Thank you !!!
 
Registered: November 09, 2010Reply With QuoteReport This Post
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-how much wvo are you working with?
-your AE process seems correct except I'm not sure on how much acid you used /ltr of oil
-If T didn't budge, there are two possabilities, caustic in the container used for AE or wet wvo. are you doing the ae process in the processor? 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-

I am using (151 L) 40 gallons. The machine I'm using is a Bio-max 150. I use it for all stages.
Afterwards its rinsed out and sits for a day to dry, and I also open the bottom drain valves to insure no water is left. I then fill it with oil, and run a drying cycle for 8 hours at 140 f before AE.

I live in Phoenix, Az and this oil has been sitting for a month prior to being ran through a centrifuge. It sits for a couple more weeks in a 55 gallon cone tank. I drain the bottom 5 gallons for inspection then dump it back into the main settling tank.

What can I do to figure this out ?
 
Registered: November 09, 2010Reply With QuoteReport This Post
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I have wvo that titrated 13-15 and tried AE using about 350 cc. of Rooto for 40 gallon batches with 3.5 gallons of methanol. The titrations wouldn't drop and adding more acid actually caused the titration to rise. The next 40 gallons of wvo I used 160 cc. of Rooto with 3.5 gallons of methanol with heat at 140 F and overnight the titration dropped to 4. So you can use to much acid. Do you run a hot plate test(HPT)? to verify the wvo is dewatered. For the methanol I use 3.5 gallons at AE and 4.5 for the base(KOH) reaction and another 1.5 gallons for the second base reaction using NaOH. I can never get full conversion (3/27) at the first base reaction. For oil titrating 36 I'd try 200-250 cc.of acid in 3.5 gallons of methanol. I think 700 cc. is too much acid.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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quote:
am I going wrong ? Does the treated oil need to sit/cool for a certain amount of time ?

Is the reactor sealed ? I had problems because my reactor didn't have a tight cover and the methanol was vaporizing out,and causing failed AE reactions. I don't think cooling will help ,in fact AE seems to work better in the 140 -160 range ,at least that's from my experiences.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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Yes it is sealed, and I havent had issues prior to this, so it came as a shock when my values didnt change at all.

What can I do to find out what happened ? Should I demeth and re titrate ?
How should I proceed with this, I cant imagine trying to do a base reaction with that high of a titration value.

Thank you
 
Registered: November 09, 2010Reply With QuoteReport This Post



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Do you have any way of checking the PH of the mix at this point? PH must be 1.5 or lower for AE to work well. you have got some contamination in this batch for sure, I suspect water since you rinsed the processor out prior to AE. the pump and plumbing are great places for water and caustic to hide.
-If this mix has been sitting for several hours , overnite is better, drain off 4 ltrs of junk from the bottom, then add 4 ltrs of methanol with 1 ml of acid per ltr in the tank. heat and mix the batch for 10 minutes then let it sit with the heat on overnite and then check T. with that high titration AE will have to be done in two stages because as the chemical reaction takes place water is created and this will stop the reaction.
-don't worry about too much acid at this point, much of it will be will leave with the drainage.
-your close to Buckeye? one of the people here who has lots of experiance processing high T trap grease presented here as buckeye biodiesel, he has conection to the buckeye sun news paper if you want to look him up. 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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my initial reaction..
you started with wet oil..a day to dry??..do you bubble air through the oil during this time?
I've waited 3-4 days heating, bubble air for oil to dry enough.

the rest of the numbers seem right. 5 gallons is around 12%..750ml of acid might be high..but not TOO high..

what to do??
if you were to wash the oil with water again..the acid would follow the water..so would the methanol..

do you have methanol recovery?? if so recovery all you can first, then wash with water.

then dry...HTP is the start of dry enough..did you test this batch using HTP first?
you do know what HTP is right?

if you can I would 2nd the looking up of Buckeye..if you read through the long sticky that I started, he helped greatly to deepen the understanding on AE processing.

Tom...Hi Smile I haven't started on my trailer yet..

-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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BF
-another way to look at this each ml of acid/ltr of oil adds about 2 points to T you added 6 ml of acid so if AE didn't work at all I would expect your T would be about 48.
-Hi Dave Email coming! 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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Bio T
I dont have any way to check ph, I will look into getting something. I will also see about getting with buckeye biodiesel. It would be great to have some locals to chat with.

I would be real suprised if water/caustic was left behind, only because the bottom drain valve was left open as well. That being said, something is definately not right, so I wont write it off.

If my T number increased to say 48 after my ae, it would indicate to much acid correct ?
If my T number stayed the same after 2 AE stages, it would indicate what ?

dkenny,
the oil passed the hot pan test, it sits for a month in the sun, and then gets run through a centrifuge at 140 f,and through a 1 micron bag filter. then it sits in a cone tank for 2 weeks before it gets to the processor.
After that it goes through a 8-10 hour drying process in the main tank @ 140f, fans on high, and with a bubbler. (this is a peace of mind process for me)

I dont have a way to recover methanol at this point. Its in the future, but first I'd really like to figure out how/what to do when these curve balls hit me.

How much water would have had to been in that oil to completely negate the ae ? Wouldnt I also have some water draining of the bottom ?

The only thing I've noticed, is the titration seems to increase with each batch, the oil is from the same source, same container per se. 12,24 , and now 36.. does the oil go bad ?

I am very thankful for the help in figuring this out. Is there a way I can use a small sample of this batch to figure out whats wrong ? I will also take a small sample down to AZ biodiesel, and see if they can offer any infomation.
 
Registered: November 09, 2010Reply With QuoteReport This Post
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quote:
Originally posted by BFoster:

Added the mixture to the oil and let recirculate for 8 hours (overnight) at 140 f.
tested and got 36t...

What am I missing ?
Your problem is that you left it mix for 8 hours. You are supposed to stop mixing after you add the acid to the oil.
 
Registered: October 04, 2010Reply With QuoteReport This Post
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quote:
If my T number stayed the same after 2 AE stages, it would indicate what

-If you where to calculate how much acid you added altogeather /ltr of oil and multiply that by 2, that would indicate the T attributed to the sulfuric acid. Sergio is right, it is important not to mix for the entire AE process because the acid (a good portion of it) doesn't get a chance to settle out and causes your T to be higher.
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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OH, well that explains a lot.

So mix it for ? 20 mins then let it sit whith heat for 8hours would that have been okay ?

Should I try that ? heat if for a couple hours ( no mix ) and see if anthing happens ?

Thank you !!!!
 
Registered: November 09, 2010Reply With QuoteReport This Post
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Turns out my T solution was bad...=(

The oil is at 3.5 !!! Thanks for all the input, it certainly has helped !!!
 
Registered: November 09, 2010Reply With QuoteReport This Post
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BF
-the titration droped to 3.5 or the first titration of T36 was in error? 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
- My final T was 3.5. I didnt save a sample of the pre AE oil, so I wont know if my actual start T value was wrong too.
 
Registered: November 09, 2010Reply With QuoteReport This Post
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don't you just hate it when its something simple..

with that much acid added your starting T was too far off..

for drying..your process sounds good..

yes oil does go bad..that's why we have AE..when the ester chains are broken from the glycerin back bone the titration goes up..these ester chains are the FFA's we test for during a 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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dkenny-
LOL, yeah it certainly got frustrating. Though its good to be stumped, it sure makes you look at your process carefully, and think about whats happening. Now I have a better understanding of something.... Wink

So thanks again for the help !!! Big Grin
 
Registered: November 09, 2010Reply With QuoteReport This Post



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You're welcome..
please don't count the number of times I made a simple mistake.. Smile

please keep us informed about you future AE results..both the good and the bad.
many others are still learning this end of BD making

-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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