Re: [Biofuel] methanol recovery/first batch results

2004-10-29 Thread rb 9 tr

--- Keith Addison [EMAIL PROTECTED] wrote:

[...]
 Quality testing

http://journeytoforever.org/biodiesel_vehicle.html#quality

One question about this testing: Aleks says, thin
layer
chromatography (tlc) can be used to determine
conversion rate and hence quality.
Has anybody done this ? 
What kind of eluent or mix is best to use for this ?

Thanks

Rainer




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Re: [Biofuel] methanol recovery/first batch results

2004-10-22 Thread Keith Addison




what kind of a methanol recovery rate can I expect once I start doing that?


Depends which stage you do it at, and what you want to do with the 
by-product. Easiest is taking back the methanol straight after 
processing, before separating the by-product, but this is inclined to 
cause a reverse reaction in the biodiesel. Still, you can get a lot 
back before that happens, especially with a vacuum.


Otherwise, about 70% of the excess methanol ends up in the glycerine 
by-product, and about 30% in the biodiesel. A simple condenser will 
get most of the 30% back from the biodiesel without too much trouble. 
As for the by-product fraction, if you have a market for potassium 
fertiliser and/or industrial-grade glycerine (about 80-90% pure) 
which makes it worth the cost and time, it's best to separate the 
by-product into it's components first, which is hard (or impossible) 
once the methanol's been removed. After separation the methanol is 
left in the glycerine fraction and can be removed then. See:

http://journeytoforever.org//biodiesel_glycsep.html
Separating glycerine/FFAs

Whether separated or not not, I'm not sure how much vacuum you'd 
need, but with heating alone the by-product or the separated 
glycerine would have to go to about 150 deg C to get most of the 
methanol back. We found it's not really economical to go much beyond 
about 105 deg C, which does get a lot back, but far from all of it. A 
better way is to use a thin-film evaporator, as Todd has recommended.


I got the product of my first conversion this morning and it looks 
straw yellow but a bit cloudy, should I let it sit to clarify or 
should I wash it?


Usually it's cloudy at first. It settles after a while. Ours is 
usually  clear by the next day.



will the cloudiness wash out?


Yes.


does that mean that my reaction is incomplete?


Not necessarily.


should I add more lye and methanol and reprocess?


A better way of finding that out is this:
Quality testing
http://journeytoforever.org/biodiesel_vehicle.html#quality


should I have titrated in the first place?


Well, I'd say yes. I still think you're starting in the wrong place. 
Up to you, of course.


Best wishes

Keith



John Guttridge


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Re: [Biofuel] methanol recovery/first batch results

2004-10-22 Thread John Guttridge


bottom, a thick white layer in the middle and a milky yellow layer on 
the top.


interestingly my siphoned off biodiesel separated again over the 
following night into a perfectly clear yellow layer on the bottom and a 
milky yellow layer on the top.


I have posted some images here:
www.lightlink.com/jonny5/biofuel/

you will have to excuse the complete lack of processing on the images, I 
don't have my tools installed on the new laptop yet.


I think that you are right that I am starting in the wrong place here. I 
am going to do another batch this afternoon using the pelly method and 
see how it works out.


John Guttridge.

Keith Addison wrote:

Hello John

what kind of a methanol recovery rate can I expect once I start doing 
that?



Depends which stage you do it at, and what you want to do with the 
by-product. Easiest is taking back the methanol straight after 
processing, before separating the by-product, but this is inclined to 
cause a reverse reaction in the biodiesel. Still, you can get a lot back 
before that happens, especially with a vacuum.


Otherwise, about 70% of the excess methanol ends up in the glycerine 
by-product, and about 30% in the biodiesel. A simple condenser will get 
most of the 30% back from the biodiesel without too much trouble. As for 
the by-product fraction, if you have a market for potassium fertiliser 
and/or industrial-grade glycerine (about 80-90% pure) which makes it 
worth the cost and time, it's best to separate the by-product into it's 
components first, which is hard (or impossible) once the methanol's been 
removed. After separation the methanol is left in the glycerine fraction 
and can be removed then. See:

http://journeytoforever.org//biodiesel_glycsep.html
Separating glycerine/FFAs

Whether separated or not not, I'm not sure how much vacuum you'd need, 
but with heating alone the by-product or the separated glycerine would 
have to go to about 150 deg C to get most of the methanol back. We found 
it's not really economical to go much beyond about 105 deg C, which does 
get a lot back, but far from all of it. A better way is to use a 
thin-film evaporator, as Todd has recommended.


I got the product of my first conversion this morning and it looks 
straw yellow but a bit cloudy, should I let it sit to clarify or 
should I wash it?



Usually it's cloudy at first. It settles after a while. Ours is usually  
clear by the next day.



will the cloudiness wash out?



Yes.


does that mean that my reaction is incomplete?



Not necessarily.


should I add more lye and methanol and reprocess?



A better way of finding that out is this:
Quality testing
http://journeytoforever.org/biodiesel_vehicle.html#quality


should I have titrated in the first place?



Well, I'd say yes. I still think you're starting in the wrong place. Up 
to you, of course.


Best wishes

Keith



John Guttridge



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Re: [Biofuel] methanol recovery/first batch results

2004-10-22 Thread Joe . Guthrie






John, I am a novice at this too so others should feel free to criticize my 
remarks.

 I would suggest you titrate.  This is not so easy at this stage because any 
free fatty acids in your fuel as you went into the base process are now
soap, that is they are neutralized with Na.To convert them back to free 
fatty acids, I have taken say 10 ml of the product, and mixed it with
vinegar strong enough to drop the pH back down to say 3 or 4. This will strip 
off the sodium.  Separate  this 10 ml of oil from the vinegar. Now you
can titrate as if it were any waste or new oil.  I think you are correct in 
assuming that you should have titrated in the first place.  If you find
that the free fatty acid is above 1 g/l equivalent NaOH then you will need to 
be careful when washing not to add much water to the first few washes.
Check out the University of Idaho process.  They use 5.5% to start out with and 
mix it up before the glycerin phase is separated off. Then settle for
as long as it takes to get clear.  But that process assumes you have the 
correct amount of NaOH or KOH added to your mix in the first place.  Since
you did not titrate first, you may not have added enough NaOH to neutralize the 
FFA's as well as catalyze the reaction.  So the reaction may not have
gone to completion. If you think that that is a possibility,  You could always 
separate the glycerin, titrate as above, add 1/4 the original methanol
and enough NaOH to both neutralize as well as catalyze. Then re-react.  This 
second product will probably not drop any glycerin unless there was a lot
of unreacted oil.

I would probably let this batch settle and make a new batch with proper 
titration.  You will learn from the new batch how to deal with the old.



   
  John Guttridge   
  [EMAIL PROTECTED] To:  [EMAIL PROTECTED]
  com cc: 
  Sent by: Subject: [Biofuel] methanol 
recovery/first batch results
  biofuel-bounces@ 
  wwia.org 
   
   
  10/21/2004 09:16 
  AM   
  Please respond   
  to biofuel   
   



what kind of a methanol recovery rate can I expect once I start doing that?

I got the product of my first conversion this morning and it looks straw
yellow but a bit cloudy, should I let it sit to clarify or should I wash
it? will the cloudiness wash out?  does that mean that my reaction is
incomplete? should I add more lye and methanol and reprocess? should I
have titrated in the first place?

John Guttridge

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Re: [Biofuel] methanol recovery/first batch results

2004-10-22 Thread Legal Eagle


downsized version ? You got a Winzip? I could fire them off in a matter of 
minutes if you like. Let me know


Luc
PS: Congrats on getting started on your way to making good quality BD.
- Original Message - 
From: John Guttridge [EMAIL PROTECTED]

To: [EMAIL PROTECTED]
Sent: Friday, October 22, 2004 1:27 PM
Subject: Re: [Biofuel] methanol recovery/first batch results


I did the quality test and it resulted in a milky white layer on the 
bottom, a thick white layer in the middle and a milky yellow layer on the 
top.


interestingly my siphoned off biodiesel separated again over the following 
night into a perfectly clear yellow layer on the bottom and a milky yellow 
layer on the top.


I have posted some images here:
www.lightlink.com/jonny5/biofuel/

you will have to excuse the complete lack of processing on the images, I 
don't have my tools installed on the new laptop yet.


I think that you are right that I am starting in the wrong place here. I 
am going to do another batch this afternoon using the pelly method and see 
how it works out.


John Guttridge.

Keith Addison wrote:

Hello John

what kind of a methanol recovery rate can I expect once I start doing 
that?



Depends which stage you do it at, and what you want to do with the 
by-product. Easiest is taking back the methanol straight after 
processing, before separating the by-product, but this is inclined to 
cause a reverse reaction in the biodiesel. Still, you can get a lot back 
before that happens, especially with a vacuum.


Otherwise, about 70% of the excess methanol ends up in the glycerine 
by-product, and about 30% in the biodiesel. A simple condenser will get 
most of the 30% back from the biodiesel without too much trouble. As for 
the by-product fraction, if you have a market for potassium fertiliser 
and/or industrial-grade glycerine (about 80-90% pure) which makes it 
worth the cost and time, it's best to separate the by-product into it's 
components first, which is hard (or impossible) once the methanol's been 
removed. After separation the methanol is left in the glycerine fraction 
and can be removed then. See:

http://journeytoforever.org//biodiesel_glycsep.html
Separating glycerine/FFAs

Whether separated or not not, I'm not sure how much vacuum you'd need, 
but with heating alone the by-product or the separated glycerine would 
have to go to about 150 deg C to get most of the methanol back. We found 
it's not really economical to go much beyond about 105 deg C, which does 
get a lot back, but far from all of it. A better way is to use a 
thin-film evaporator, as Todd has recommended.


I got the product of my first conversion this morning and it looks straw 
yellow but a bit cloudy, should I let it sit to clarify or should I wash 
it?



Usually it's cloudy at first. It settles after a while. Ours is usually 
clear by the next day.



will the cloudiness wash out?



Yes.


does that mean that my reaction is incomplete?



Not necessarily.


should I add more lye and methanol and reprocess?



A better way of finding that out is this:
Quality testing
http://journeytoforever.org/biodiesel_vehicle.html#quality


should I have titrated in the first place?



Well, I'd say yes. I still think you're starting in the wrong place. Up 
to you, of course.


Best wishes

Keith



John Guttridge



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Re: [Biofuel] methanol recovery/first batch results

2004-10-22 Thread Legal Eagle


before each go of it. Once you have your catalyst amount determined re-do 
the titration to be sure you got it right the first time and use the Better 
Titration method.

http://journeytoforever.org/biodiesel_make2.html#bettertitrate
I have found that a VERY good electronic PH meter and scale are invaluable. 
They help eliminate those two areas of potential variants.
The other sore spot I found to be heat. The processing heat should be 55C 
(130F), and not considerably lower. A good thermometer helps.
http://journeytoforever.org/biodiesel_make2.html#lye All about lye and the 
next one too How much lye gives you the groundwork for either NaOH or KOH 
as a catalyst per volume of mathanol.
I have not attempted the two stage method yet nor am I intending to until 
the one stage has become perfectly clear and I am getting consistant 
positive results. Everything in it's time.


Luc

- Original Message - 
From: [EMAIL PROTECTED]

To: [EMAIL PROTECTED]
Sent: Friday, October 22, 2004 2:33 PM
Subject: Re: [Biofuel] methanol recovery/first batch results


John, I am a novice at this too so others should feel free to criticize my 
remarks.


I would suggest you titrate.  This is not so easy at this stage because any 
free fatty acids in your fuel as you went into the base process are now
soap, that is they are neutralized with Na.To convert them back to free 
fatty acids, I have taken say 10 ml of the product, and mixed it with
vinegar strong enough to drop the pH back down to say 3 or 4. This will 
strip off the sodium.  Separate  this 10 ml of oil from the vinegar. Now you
can titrate as if it were any waste or new oil.  I think you are correct in 
assuming that you should have titrated in the first place.  If you find
that the free fatty acid is above 1 g/l equivalent NaOH then you will need 
to be careful when washing not to add much water to the first few washes.
Check out the University of Idaho process.  They use 5.5% to start out with 
and mix it up before the glycerin phase is separated off. Then settle for
as long as it takes to get clear.  But that process assumes you have the 
correct amount of NaOH or KOH added to your mix in the first place.  Since
you did not titrate first, you may not have added enough NaOH to neutralize 
the FFA's as well as catalyze the reaction.  So the reaction may not have
gone to completion. If you think that that is a possibility,  You could 
always separate the glycerin, titrate as above, add 1/4 the original 
methanol
and enough NaOH to both neutralize as well as catalyze. Then re-react.  This 
second product will probably not drop any glycerin unless there was a lot

of unreacted oil.

I would probably let this batch settle and make a new batch with proper 
titration.  You will learn from the new batch how to deal with the old.





 John Guttridge
 [EMAIL PROTECTED] To:  [EMAIL PROTECTED]
 com cc:
 Sent by: Subject: [Biofuel] methanol 
recovery/first batch results

 biofuel-bounces@
 wwia.org


 10/21/2004 09:16
 AM
 Please respond
 to biofuel




what kind of a methanol recovery rate can I expect once I start doing that?

I got the product of my first conversion this morning and it looks straw
yellow but a bit cloudy, should I let it sit to clarify or should I wash
it? will the cloudiness wash out?  does that mean that my reaction is
incomplete? should I add more lye and methanol and reprocess? should I
have titrated in the first place?

John Guttridge

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re: [Biofuel] methanol recovery/first batch results

2004-10-21 Thread DHAJOGLO

I got the product of my first conversion this morning and it looks straw
yellow but a bit cloudy, should I let it sit to clarify or should I wash
it? 

You will need to do your meth recovery before you wash it as washing will 
remove the meth into the wash water where its harder to recover.

will the cloudiness wash out?

that cloudiness is a number of things, soaps, some glycerol.  If you aren't 
doing meth recovery then I would just let it settle for a day or so (longer if 
you can).  It allows small quantities of glycerol to settle out and makes for 
easier washing.  If you are recovering then run your recovery then let it set.  

should I have titrated in the first place?

You should follow the instructions for which every process you're using.  
Titration is a useful tool but doesn't necessarly make your process work any 
better or worse unless you understand how to intrepret and apply the data.


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