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hook
-yes, that made a lot of sense to me as well, I am processing right now, and will post the results. next step dump all my electric heating elements Big Grin 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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Hello, Just skimmed thru this thread and admittedly haven't had time to read every post but; what about silica gel, stir it in within a porous bag, pull out, sun dry and reuse? It shouldn't absorb oil and is pH neutral.


 
Registered: June 24, 2009Reply With QuoteReport This Post
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I'm closer to processing his way instead of the 80/20..if anything I'll put way more methanol and KOH in the second stage..many times its 1000grams and 2-3 gallons methanol in a batch.. I don't what 27/3 issues..so this might be over kill..so..I recover the methanol.
now if I could figure out how to recover the excess KOH..

I would like to see the overall cost of using AE lowered..for all T's of oil.

-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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Dave Hook
-just finished the first phase of the base process. 160 ltr batch. 14 ltr for acid stage, withdraw (drain 14ltrs after acid stage) base process with 24ltr methanol and 1600gr koh (T.75 +9) just checked and pass 3/27 not 4/27 so will settle and drain repo in the morning with 10ml/ltr methanol and 1 gr koh per ltr to force the reaction further to the right. Another tid bit , Rex said to keep the methanol for the 3/27 test in the freezer, mono and di glycerides do not disolve well in cold methanol. could we have another change in the process? Tom
-oh ya, staring t of this oil was 4.5

This message has been edited. Last edited by: Biotom,


" 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 Double D:
dkenny,
I checked the math and the T x 4.3 is keeping with a 6:1 molar ratio.

Would it also be beneficial to keep the H2SO4:FFA at a set molar ratio?

I took the liberty of working up a molar ratio for T-3*.15, where T = 20
At a titration of 20ml KOH this work out to a molar ratio of 7.44:1, FFA to H2SO4.

So the math works out to
T x.546=(___/100)x W =___g/282=___m FFA/7.44=___m H2SO4 x 98.08 =___/1.84= ___ml H2SO4 needed per Liter.

W= weight of one Liter of your oil.
T= titration in ml KOH


Another simpler way would to claculate at a FFA:H2SO4 molar ratio would be,
7.44:1 = Titration /7.84 = .15 multiplier
11.125:1 = Titration /11.76 = .1 multiplier
22.25:1 = Titration / 23.5 = .05 multiplier
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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Double D,

thanks for working the formula's through. it helps to keep the math simpler.

My next batch..
65 gallons or 246 L.
Titration 44

acid multi 0.08
methanol I'm going to try the T*4.3 if the tank has room..

acid per ml
44-3*0.08 = 41*0.08= 3.28ml/liter * 246 = 806.88 I'm going to use 810 mls..easier to measure
methanol
44 * 4.3 = 189.2mls/liter * 246 = 46543ml or 46.5 liters or 12.3 gallons..so it'll fit in the tank.
I'll definately save this for methanol recovery.

start time will be around 4pm today

just thought I add some thoughts about what I hope to have happen.
1. a lower ending titration. T of 3.28*2.25 = 7.38 or less..this would indicate a complete esterification reaction.
2. higher yield.. the last 2 batches of this yield we terrible.
3. a problem that might come up it trying to drain..this mix might float.


here's a suprise..
after 1-1.5 hrs the titration is now T30..a 14 point drop in 1 hr..if it does that for 3 more hours..SmileSmile

-dkenny

This message has been edited. Last edited by: 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:
Originally posted by dkenny:
Double D,

thanks for working the formula's through. it helps to keep the math simpler.

My next batch..
65 gallons or 246 L.
Titration 44

acid multi 0.08
methanol I'm going to try the T*4.3 if the tank has room..

acid per ml
44-3*0.08 = 41*0.08= 3.28ml/liter * 246 = 806.88 I'm going to use 810 mls..easier to measure
methanol
44 * 4.3 = 189.2mls/liter * 246 = 46543ml or 46.5 liters or 12.3 gallons..so it'll fit in the tank.
I'll definately save this for methanol recovery.

start time will be around 4pm today

just thought I add some thoughts about what I hope to have happen.
1. a lower ending titration. T of 3.28*2.25 = 7.38 or less..this would indicate a complete esterification reaction.
2. higher yield.. the last 2 batches of this yield we terrible.
3. a problem that might come up it trying to drain..this mix might float.


-dkenny


Assuming the reaction go to 90% completion.
You should be left with approximately,
12.6ml H2O
100.67ml CH3OH
3.18ml H2SO4

This would give you a SG of .843g/ml.

This post has been edited to correct the SG.

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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Double D,

that would be great. I assume those numbers are per liter.

that mean the mix would sink like a stone since oil it around .92 SG..Smile

time will tell for sure.

I would need to drain out about 7.3 gallons..slight more than 1/2 of the methanol I started with...I would expect this since the titration is so high.

-dkenny

update my batch in process
so far it looks more methanol is working great
initial T 44
1.5 hrs T 30
5.5 hrs T 15
24hrs T 10--update 8.15...oops this is not 24 hrs but 12..Smile

This message has been edited. Last edited by: 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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It does sound encouraging but I goofed up the math. Mad It should be a SG of .843g/ml.
That's one reason I like to show the formulas for my answers, I make mistakes. Sorry.
I should add that those calculations are assuming that 90% of the FFA is converted into methyl esters. It seems to me though that there is likely hood that 90+% of the FFA could be converted but not all into methyl ester. Since there are undoubtedly alot of Mono's and Di's in there, some of the FFA could just be added back to the mono's and Di's. This would still create the same amount of H2O but not consume as much CH3OH which will lower the SG of the mix a little further.
Assuming that half of the FFA are converted to methyl esters and half are added back to glycerides, the SG would only drop to .822g/ml

I'll try to do some calculations to see what molar ratio of H2SO4 to CH3OH is needed to raise the SG to say 1.1 or so.

It looks like this batch of yours has a molar ratio of 16.66FFA:1H2SO4.
I'll go back up and edit the other post.

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:
Originally posted by Double D:
Using your 6:1 molar ratio of Methanol to FFA it appears that you would need a 10:1 molar ratio of Methanol to Sulfuric to raise the SG to .929g/ml. Eek
At a titration of 44ml/KOH, this works out to needing 25ml H2SO4 per liter of oil. Eek This is calculated using the following:
Oleic Acid at 282g/m
CH3OH at 32.05g/m SG .792g/ml
H2SO4 at 98.08g/m SG 1.84g/ml
H2O at 18g/m SG 1g/ml
1L oil at 920g
This is assuming 50% of the FFA is converted to methyl ester and 50% bound to glycerides = 100% conversion.

C x .546/100 x 920 = A/282 = B

A= g FFA
B= moles FFA
C= Titration in ml KOH

((44 x .546)/100)x920 = 221.02g/282 = .784 moles FFA

6:1 molar ratio of Methanol to FFA = 6 x .784 = 4.704m CH3OH
10:1 molar ratio of Methanol to H2SO4 = 4.704/10 = .470m H2SO4

H2SO4 .470m x 98.08 = 46.098g
4.704m CH3OH = 4.704 x 32.05 = 150.763g CH3OH
1/2 of the FFA being converted to methyl esters = .784m/2 = .392m x 32.05 = 12.56g
150.763 - 12.56g = 138.203g CH3OH left in the mix unconverted.
.784m of converted FFA converted = .784m H2O produced x 18g = 14.112g H2O

CH3OH = 138.203g/.792 = 174.499ml
H2SO4 = 46.098g/1.84 = 25.053ml
H2O = 14.112g/1 = 14.112ml

Totals 198.413g/213.614ml = .929 SG
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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Double D,
so it get it to sink I would use less than 6:1 molar for the methanol. for higher titration oils this might be a requirement. if this batch gives 90% or higher yield, then I think draing from the top would a good requirement. should be too hard to design in from the start.

I my batch as of 18hrs is T9.. I'll check again at 24hrs..

-dkenny

update on my batch
in 24 hrs it went from T44 to T7
I'm going to let it run for another 12 hrs because I'm too tired to mess with it tonight. tomorrow I check the titration again. its already at the calculated minimium, but can it go lower. several people on this thread have had it happen..why? then I'll let it settle..I drain some from the bottom and check the titration. if Double D is correct in he's math this mix with float. so the titration at the bottom will be just the oil. of course I'll remix and use that titration for starting the base stages.

This message has been edited. Last edited by: 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
will you look for floating crud before mixing and going on to the base stage? My first AE try floated and I removed it and replaced the volume with methanol. It was only T 4.8 oil though.
I haven't had time to work on the T 85 stuff yet. It is hay season and I'm dodging storms etc. Tom2


Eating fried foods is fuel-ish behavior.

 
Location: Cerrillos, NM | Registered: July 25, 2009Reply With QuoteReport This Post



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akwrench,

with this batch I expect the mix to float..I'm planning on removing it from the top.

with you T4.5 batch there's no need to remove the mix between the acid and base stages. the other stuff the T85..you need to drain between..you might need more than one acid stage.

I haven't checked my batch yet today. still waking up and drinking coffee Smile

update ->
ending T before drainging is 6..Smile this is after about 40 of processing. its now settling then I'll drain.

here's a twist..the mix sank.. I just drain about6 gallons from the bottom. I think I might have an answer as to why. Potassium Sulfate(K2SO4)..or KOH + H2SO4 -> i think does get created and dissolves in water. making the density of the water/methanol/acid/K2SO4 mix higher. I just wikied it and yes it white and dissolves in water. the white crud at the bottom that some of use see..hum..


-dkenny

This message has been edited. Last edited by: 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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Where could the potassium come from?
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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I'm guessing left over the last batch. stuff in the oil( but might make it something else besides K2SO4). I just know something increase the SG of the mix and it sank.

yield for this batch is better around 60 out of 65 gallons or 92%..I happier with this result than the prior 2.

-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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Anyone willing to help with a problem? Got 6inches of butter-like substance on top of batch after acid treat then reaction....No glycerin.
 
Location: Upper South Carolina | Registered: December 11, 2007Reply With QuoteReport This Post
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flyinit

-What was the T, was the ae process carried out hot or cold,how much time, how much methanol, explain your wvo drying proceedure. 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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Thanks,

500 gal reactor, 20gpm pump. 3-4500 watt emersion elements in a circutated manifold for heat.

I think this will boil down to how I introduced the methoxide...

I collect WVO and let settle for several weeks. Pump from top of settle tanks into processor. This was a 210 gallon batch. circulate & heat to 135 degrees while spraying back through drying nozzles for 8 hours to dry. next day, starting titration is 9.8 NAOH. Recirculate & heat oil to 135 degrees. Use formula (titration - 3 x .2)to determine H2SO4 (1.36 ml/l). Introduced 25 gallons methanol to hot oil while circulating. Then introduced 1081ml H2SO4 98% to oil/meth mix while circulating. After 5 hours, titration was 4.1 and had stopped moving. Immediately mixed 6042 grams NAOH with 19 gallons methanol and introduced to batch while circulating. Mixed for 6 hours in sealed reactor. let settle for a day. Opened reactor and there was 6 inches of butter-like glop on top, unprocessed oil on bottom. No glycerin on bottom.



I have never seen the butter-like substance before, it is not like an emulsion. It is actually hard.

Here is what I think happened. I had just modified the processor so I can dump methoxide from the top, instead of slowly introducing it to the wvo at he suction side of the pump via an intake manifold. It seems that methoxide never mixed with the wvo...but what is the solid mass on top?

Any suggestions on how to fix the mess would be appreciated.
 
Location: Upper South Carolina | Registered: December 11, 2007Reply With QuoteReport This Post



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flyinit
-when you say hard top layer, then I will assume the reator was allowed to cool? (layer = soap)
-I just calculated, it takes about 10.5 min to circ the batch once. I had problems with my processing, and I was circulating once every 6 min. even with slow methoxid injection it wasn't gettiner done. So first, it seems that mixing is one problem.
-T stopped lowering after 5 hr on T9.5 (naoh) wvo. this will not happen if the wvo is dry! Water stops ae process dead in it's tracks. so as it works, it creates even more water and then take this to the base process and add the remaining methanol. the methanol that was added for the ae process will now be contaminated with water. so there is insufficiant methanol strength to push the base process to completion, and lots of water, caustic and ffa's to make soap!
- what to do now grab a sample and do a test batch, starting with 1ml methanol and 1 gram of naoh / ltre of wvo and see what it takes to complete this reaction. then calculate this amount and reprocess. You can remove the hard soap prior to reprocessing, this should make washing a little easier.
-When I dry wvo, I follow a similar process, exept 145f, and 8 hrs is fine for the base process, BUT when doing ae I dry for 24 hr. 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, would it be a problem not draining off the methanol/acid/water layer than forms on the bottom or top of the BD?
 
Registered: March 02, 2009Reply With QuoteReport This Post
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