RE: [Biofuel] Cold Weather Processing
Sory, I'm two days behind. Keith, I did graduate from college with a BA in Chemistry and I did do my senior thesis research on biodiesel. I didn't get anywhere near what I wanted to get accomplished with my project since the school I went to had virtually no working instruments to test with. I started with the straight forward biodiesel reaction with methanol and vegetable oil with NaOH catalyst and then tried a couple variations with ethanol. I also tried a couple ether-alcohols 1-methoxy-2-ethanol and 2 methoxy-ethanol. In those reactions, the glycerine combined with the alcohol instead of the fatty acid, and I was left with soap as the other product. It seemed that the reaction was temperature dependent as when the temperature for those 2 reactions was above 70 degrees celsius, there was definite glycerine present as the color of the reaction mix became a dark amber, but as the temperature dropped in the deparation vessel the brown color disappeared and became a milky cloudy color. Now, the only instrument available to me in the lab was NMR which wasn't very helpful to me other than to tell me qualitatively what I had, but not the purity. I was hoping to do some HPLC tests to see what kind of reaction % I was getting. I also tried using isopropanol which didn't work with the NaOH or KOH. I reacted Na metal with the isopropanol (I was using 99.5% pure and not rubbing alcohol) and a precipitate formed since the Na metal did not react vigorously enough before the oxygen in the air reacted to form NaOH. I tried potassium metal which reacted readily with the alcohol and using the potassium isopropoxide in isopropanol solution I had created as a catalyst, I was able to get a reaction just as in the complex ether-alcohols but the end result was similar... when the temperature dropped to room temperature in the separation vessel, the glycerine disappeared and I ended up with an unseparated product. I found also that using sodium metal (reacting on a mole-to-mole basis) with ethanol to get the same sodium concentration as with lye and this was the most effective route for me overall. There was no problem with separation and since there was no water produced in the reaction (the byproduct would be a sodium salt of glycerine) there was no emulsion when washing as I had experienced in the other tests. I don't know how feasible it would be to use sodium metal though, since it is highly reactive with water. I didn't have the time to try more complex tests than these, and was thoroughly disappointed that I couldn't do more instrumental analysis to find the purity of the product I produced. I should also note that you can purchase sodium ethoxide or sodium methoxide in salt form as well. I wish I knew where I kept the paper I found on the subject but there was a university study that showed that the use of sodium methoxide or sodium ethoxide was superior when working with pure ethanol, but that potassium ethoxide and methoxide did not yield a good separation... this I don't know why. Like I said, there was much more I wish I could have done, and I wish I could get in to the U of Idaho to work on biodiesel as a graduate student, but since they only accept 10 graduates (not all from the US of course) and I could have used a few extra points on my GPA, I'm not going to bother applying. What you did get done is interesting enough. I can see why you were disappointed, but on the other hand, I think any of us old farts around here might tell you it might be too soon for that. These things can have an odd way of working out in the end. Right now I am working a job that has nothing to do with what I want to do, but hopefully after I put in a couple years, I can get a better idea of what I want to do with my life. That's no bad plan. That's what I did (not that that necessarily means it's a good plan!). I had no idea what I wanted to do with myself, other than that it wasn't what my elders and betters wanted me to do. Remember The Graduate? It was those days: Plastics! Huh? So I just did whatever came to hand, this for a couple of years, then that for another, and so on - I had five or six jobs before I finally joined a newspaper, for better or for worse (both!). But I never regretted any of those previous jobs, it all helped a lot. You have a farming background, you know about sustainable farming, you studied chemistry and you know a lot about biofuels. That sure makes for some interesting combinations. I think the world needs people like you, even if it hasn't realised it yet. Hang in there Jeff, I'm sure you'll find your path, or it will find you. Regards, and good luck Keith Regards, Jeff Original Message Follows From: Keith Addison [EMAIL PROTECTED] Reply-To: [EMAIL PROTECTED] To: [EMAIL PROTECTED] Subject: RE: [Biofuel] Cold Weather Processing Date: Sun, 10 Oct 2004 22:18:13 +0900 Hello Jeff I'm
Re: [Biofuel] Cold Weather Processing
Did you ever try Hydroxides of other active metals, say lithium ? Has anyone? Greg H. - Original Message - From: Legal Eagle [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Saturday, October 09, 2004 06:54 Subject: [Biofuel] Cold Weather Processing G'day; Snip Better system yet? Use potassium hydroxide and don't worry about theabove time-consuming PITA (Pain In The Anatomy). As still somewhat of a beginner at this BD making stuff I have a whack of NaOH that I got from a chem supply house that now has to be used, although once I have thorougly pefected using my system and understanding it's ups and downs to where I ma comfortable with it's nuances I will be looking into KOH as a catalyst. That will be for the next season, as this one winds down due to cold and I don't have the with all to properly insulate the pump house, although I will be using the off-season to do that as well as set up the secondary settling tank in preparation for a full and rewarding production season next year. The off-season time will also be used to stock up on things like, methanol and WVO (it's pretty good stuff I get from the Chinese Restaurant and I want to get ahead of it for next year), and insulating the pump house which will allow me to get going earlier than if I only wait for it to be warm enough in the Spring. Ordering some WintronXC30 is also on the list for early Spring use and also for next winters' BD experience. It is too bad too as the Benz REALLY likes running on B100, and it iwll do so once weather and the ability to process permits. Who knows, maybe it will be sooner rather than later, but one thing certain, I will be working at it. Luc ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: [Biofuel] Cold Weather Processing
mole of reagent. Roughly a couple of bucks for a mole of sodium, 15 bucks for lithium and 40 for potassium Greg Harbican wrote: Did you ever try Hydroxides of other active metals, say lithium ? Has anyone? Greg H. - Original Message - From: Legal Eagle [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Saturday, October 09, 2004 06:54 Subject: [Biofuel] Cold Weather Processing G'day; Snip Better system yet? Use potassium hydroxide and don't worry about theabove time-consuming PITA (Pain In The Anatomy). As still somewhat of a beginner at this BD making stuff I have a whack of NaOH that I got from a chem supply house that now has to be used, although once I have thorougly pefected using my system and understanding it's ups and downs to where I ma comfortable with it's nuances I will be looking into KOH as a catalyst. That will be for the next season, as this one winds down due to cold and I don't have the with all to properly insulate the pump house, although I will be using the off-season to do that as well as set up the secondary settling tank in preparation for a full and rewarding production season next year. The off-season time will also be used to stock up on things like, methanol and WVO (it's pretty good stuff I get from the Chinese Restaurant and I want to get ahead of it for next year), and insulating the pump house which will allow me to get going earlier than if I only wait for it to be warm enough in the Spring. Ordering some WintronXC30 is also on the list for early Spring use and also for next winters' BD experience. It is too bad too as the Benz REALLY likes running on B100, and it iwll do so once weather and the ability to process permits. Who knows, maybe it will be sooner rather than later, but one thing certain, I will be working at it. Luc ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/ -- -- Bob Allen,http://ozarker.org/bob -- - The modern conservative is engaged in one of Man's oldest exercises in moral philosophy; that is, the search for a superior moral justification for selfishness JKG --- [This E-mail scanned for viruses by Declude Virus] ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
[Biofuel] Cold Weather Processing
The addition of glycerine to the BD being washed has caused some problems. Excatly how mush gly is getting it there is hard to tell, but it is making things difficult. The wash by oscillating sprinkler system works very well, but it is a little violent and that doesn't seem to sit well with the glyc and it turns out a layer of very thick soup that won't break, so I have to empty the wash tank, BD first via the standpipe, and then clean out the wash tank completely before re-introducing the BD. Once that is done there are no more probs, except that a portion of the yield has been diminished. Of course, when dealing with colder temps and unheated surroundings, like where I have my set up, it might be a good idea to simply re-heat the lot using the reactor's heater and then firing up the pump, mixing everything back together to be sure no hardened glycerine has stayed on the bottom and then letting it settle back out for a few hours and drain it once and then again a bit later, although that might just start the porblem all over again. The best solution is a seperate settling tank or using KOH instead of the NaOH, or better still, house the reactor is a heated space when available. During the winter months I am planning on insulating the building my reactor is in as well as getting that secondary settling tank set up properly. I learned from the creation of the pre-heat tank about things to avoid, like 1/2 inch plumbing, and placing the heater too high in the tank, so that this time those errors won't be repeated. The heater element goes about 2 inches (5cm) off the bottom of the tank, that way it won't be exposed should a small amount of product be needed to be warmed up. 3/4 inch plumbing everywhere except the methoxide delivery system where 1/2 inch is plenty. For having my reactor finished only in the second week of August and already having produced hundreds of liters I believe to be a fairly good start. The Benz has gone on vacations with B100 in the tank on the way up and a good portion of the way back. It is still now running on B100, and today all those warnings about the filters clogging from all the dirty fuel deposits came true. Just before leaving on holidays I had the car's valves adjusted, all filters, oil and fuel changed for brand new MB parts and only today does it crap out on me,ha! Tomorow is replace the fuel filters day. It is funny because the fuel filter hasn't so much as a tiny scratch on it and it is useless. BD cleans ! It is with great remorse that I will have to shut down production for the winter, but then it will give me time to get it together for next year. I am finding that my one good WVO supplier isn't able to keep up with me so that will be on the list of things to do too. The organic farmer today asked if he should buy a biodiesel truck, so we all know where THAT is going huh ? I make the fuel, he uses it to help run his organic farm that produces food the way it is supposed to be done. Win, win. Luc ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
RE: [Biofuel] Cold Weather Processing
biodiesel reaction, if adding the water before removing as much glycerine as possible be a cause for some of the problems with separation and emulsions since there could be some extraneous reactions or possible reverse reactions going on in the mix? Also, in my experience, if you can get ahold of sodium methoxide or ethoxide (or if you can make it yourself using sodium metal reacted with ethanol or methanol) gives a much better separation of the biodiesel from the glycerine and the glycerine is much thicker. I would suggest that if you have trouble with separation, perhaps replacing as little as 25% of the NaOH or KOH used with the ethoxide salt (on a molar basis) and seeing how that works for you - adding more or less by trial and error until you get a satisfactory result. Also, using sodium ethoxide as a catalyst makes the use of ethanol instead of methanol as the alcohol more feasible - (of course, that is if you can find the salt or are willing to play with sodium metal - I'd say potassium metal is way too dangerous outside of a lab environment) most university research data shows that to use ethanol as the alcohol of choice you need an excess of almost 200% ethanol meaning 3x the amount to finish the reaction, and then the excess ethanol causes the glycerine to not separate out and you get nothing but a mess... Jeff Original Message Follows From: Legal Eagle [EMAIL PROTECTED] Reply-To: [EMAIL PROTECTED] To: [EMAIL PROTECTED] Subject: [Biofuel] Cold Weather Processing Date: Sat, 9 Oct 2004 20:15:53 -0400 The addition of glycerine to the BD being washed has caused some problems. Excatly how mush gly is getting it there is hard to tell, but it is making things difficult. The wash by oscillating sprinkler system works very well, but it is a little violent and that doesn't seem to sit well with the glyc and it turns out a layer of very thick soup that won't break, so I have to empty the wash tank, BD first via the standpipe, and then clean out the wash tank completely before re-introducing the BD. Once that is done there are no more probs, except that a portion of the yield has been diminished. Of course, when dealing with colder temps and unheated surroundings, like where I have my set up, it might be a good idea to simply re-heat the lot using the reactor's heater and then firing up the pump, mixing everything back together to be sure no hardened glycerine has stayed on the bottom and then letting it settle back out for a few hours and drain it once and then again a bit later, although that might just start the porblem all over again. The best solution is a seperate settling tank or using KOH instead of the NaOH, or better still, house the reactor is a heated space when available. During the winter months I am planning on insulating the building my reactor is in as well as getting that secondary settling tank set up properly. I learned from the creation of the pre-heat tank about things to avoid, like 1/2 inch plumbing, and placing the heater too high in the tank, so that this time those errors won't be repeated. The heater element goes about 2 inches (5cm) off the bottom of the tank, that way it won't be exposed should a small amount of product be needed to be warmed up. 3/4 inch plumbing everywhere except the methoxide delivery system where 1/2 inch is plenty. For having my reactor finished only in the second week of August and already having produced hundreds of liters I believe to be a fairly good start. The Benz has gone on vacations with B100 in the tank on the way up and a good portion of the way back. It is still now running on B100, and today all those warnings about the filters clogging from all the dirty fuel deposits came true. Just before leaving on holidays I had the car's valves adjusted, all filters, oil and fuel changed for brand new MB parts and only today does it crap out on me,ha! Tomorow is replace the fuel filters day. It is funny because the fuel filter hasn't so much as a tiny scratch on it and it is useless. BD cleans ! It is with great remorse that I will have to shut down production for the winter, but then it will give me time to get it together for next year. I am finding that my one good WVO supplier isn't able to keep up with me so that will be on the list of things to do too. The organic farmer today asked if he should buy a biodiesel truck, so we all know where THAT is going huh ? I make the fuel, he uses it to help run his organic farm that produces food the way it is supposed to be done. Win, win. Luc ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/ _ Donât just search. Find. Check
Re: [Biofuel] Cold Weather Processing
incomplete rection, the problem is that not all the glycerine is draining once the settling time is done and that glycerine is getting mixed with the BD when it is being transfered to the wash tank and that is what is causing trouble. During the warmer months of summer this problem did not exist as the reactor was able to hold it's heat but with the overnight dropping temps it has bot done so well. The solutions are fairly simple; insulate the structure and put a small heater on a timer and/or use KOH instead of the NaOH. I have absolutely zero science knowledge (except what I have learned doing this)so I will not be experimenting with new and potentially dangerous catalyst bases, that is best left to the pros :) When the time comes and I feel comfortable enough, once having moved up to KOH as a catalyst and things are going reasonably well then I would like to go the two stage method route but not before. Call me chicken s#^t, but I prefer to err on the side of caution and go at it methodically. Luc - Original Message - From: Jeff Welter [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Sunday, October 10, 2004 4:46 AM Subject: RE: [Biofuel] Cold Weather Processing I'm wondering if since water present in small amounts can impede the biodiesel reaction, if adding the water before removing as much glycerine as possible be a cause for some of the problems with separation and emulsions since there could be some extraneous reactions or possible reverse reactions going on in the mix? Also, in my experience, if you can get ahold of sodium methoxide or ethoxide (or if you can make it yourself using sodium metal reacted with ethanol or methanol) gives a much better separation of the biodiesel from the glycerine and the glycerine is much thicker. I would suggest that if you have trouble with separation, perhaps replacing as little as 25% of the NaOH or KOH used with the ethoxide salt (on a molar basis) and seeing how that works for you - adding more or less by trial and error until you get a satisfactory result. Also, using sodium ethoxide as a catalyst makes the use of ethanol instead of methanol as the alcohol more feasible - (of course, that is if you can find the salt or are willing to play with sodium metal - I'd say potassium metal is way too dangerous outside of a lab environment) most university research data shows that to use ethanol as the alcohol of choice you need an excess of almost 200% ethanol meaning 3x the amount to finish the reaction, and then the excess ethanol causes the glycerine to not separate out and you get nothing but a mess... Jeff Original Message Follows From: Legal Eagle [EMAIL PROTECTED] Reply-To: [EMAIL PROTECTED] To: [EMAIL PROTECTED] Subject: [Biofuel] Cold Weather Processing Date: Sat, 9 Oct 2004 20:15:53 -0400 The addition of glycerine to the BD being washed has caused some problems. Excatly how mush gly is getting it there is hard to tell, but it is making things difficult. The wash by oscillating sprinkler system works very well, but it is a little violent and that doesn't seem to sit well with the glyc and it turns out a layer of very thick soup that won't break, so I have to empty the wash tank, BD first via the standpipe, and then clean out the wash tank completely before re-introducing the BD. Once that is done there are no more probs, except that a portion of the yield has been diminished. Of course, when dealing with colder temps and unheated surroundings, like where I have my set up, it might be a good idea to simply re-heat the lot using the reactor's heater and then firing up the pump, mixing everything back together to be sure no hardened glycerine has stayed on the bottom and then letting it settle back out for a few hours and drain it once and then again a bit later, although that might just start the porblem all over again. The best solution is a seperate settling tank or using KOH instead of the NaOH, or better still, house the reactor is a heated space when available. During the winter months I am planning on insulating the building my reactor is in as well as getting that secondary settling tank set up properly. I learned from the creation of the pre-heat tank about things to avoid, like 1/2 inch plumbing, and placing the heater too high in the tank, so that this time those errors won't be repeated. The heater element goes about 2 inches (5cm) off the bottom of the tank, that way it won't be exposed should a small amount of product be needed to be warmed up. 3/4 inch plumbing everywhere except the methoxide delivery system where 1/2 inch is plenty. For having my reactor finished only in the second week of August and already having produced hundreds of liters I believe to be a fairly good start. The Benz has gone on vacations with B100 in the tank on the way up and a good portion of the way back. It is still now running on B100, and today all those warnings about
RE: [Biofuel] Cold Weather Processing
I'm wondering if since water present in small amounts can impede the biodiesel reaction, if adding the water before removing as much glycerine as possible be a cause for some of the problems with separation and emulsions since there could be some extraneous reactions or possible reverse reactions going on in the mix? Have a look at this: http://infoarchive.net/sgroup/BIOFUEL/34062/ This is the glycerine wash step from Optimization of a Batch Type Ethyl Ester Process by the University of Idaho: http://journeytoforever.org/biofuel_library/ethyl_esters.html Ethyl Ester Process Also, in my experience, if you can get ahold of sodium methoxide or ethoxide (or if you can make it yourself using sodium metal reacted with ethanol or methanol) gives a much better separation of the biodiesel from the glycerine and the glycerine is much thicker. I would suggest that if you have trouble with separation, perhaps replacing as little as 25% of the NaOH or KOH used with the ethoxide salt (on a molar basis) and seeing how that works for you - adding more or less by trial and error until you get a satisfactory result. Also, using sodium ethoxide as a catalyst makes the use of ethanol instead of methanol as the alcohol more feasible - (of course, that is if you can find the salt or are willing to play with sodium metal - I'd say potassium metal is way too dangerous outside of a lab environment) most university research data shows that to use ethanol as the alcohol of choice you need an excess of almost 200% ethanol meaning 3x the amount to finish the reaction, and then the excess ethanol causes the glycerine to not separate out and you get nothing but a mess... Jeff Are you still studying Jeff? How did your senior research project/thesis go last year? Did it focus on biodiesel as you were planning? Regards Keith Original Message Follows From: Legal Eagle [EMAIL PROTECTED] Reply-To: [EMAIL PROTECTED] To: [EMAIL PROTECTED] Subject: [Biofuel] Cold Weather Processing Date: Sat, 9 Oct 2004 20:15:53 -0400 The addition of glycerine to the BD being washed has caused some problems. Excatly how mush gly is getting it there is hard to tell, but it is making things difficult. The wash by oscillating sprinkler system works very well, but it is a little violent and that doesn't seem to sit well with the glyc and it turns out a layer of very thick soup that won't break, so I have to empty the wash tank, BD first via the standpipe, and then clean out the wash tank completely before re-introducing the BD. Once that is done there are no more probs, except that a portion of the yield has been diminished. Of course, when dealing with colder temps and unheated surroundings, like where I have my set up, it might be a good idea to simply re-heat the lot using the reactor's heater and then firing up the pump, mixing everything back together to be sure no hardened glycerine has stayed on the bottom and then letting it settle back out for a few hours and drain it once and then again a bit later, although that might just start the porblem all over again. The best solution is a seperate settling tank or using KOH instead of the NaOH, or better still, house the reactor is a heated space when available. During the winter months I am planning on insulating the building my reactor is in as well as getting that secondary settling tank set up properly. I learned from the creation of the pre-heat tank about things to avoid, like 1/2 inch plumbing, and placing the heater too high in the tank, so that this time those errors won't be repeated. The heater element goes about 2 inches (5cm) off the bottom of the tank, that way it won't be exposed should a small amount of product be needed to be warmed up. 3/4 inch plumbing everywhere except the methoxide delivery system where 1/2 inch is plenty. For having my reactor finished only in the second week of August and already having produced hundreds of liters I believe to be a fairly good start. The Benz has gone on vacations with B100 in the tank on the way up and a good portion of the way back. It is still now running on B100, and today all those warnings about the filters clogging from all the dirty fuel deposits came true. Just before leaving on holidays I had the car's valves adjusted, all filters, oil and fuel changed for brand new MB parts and only today does it crap out on me,ha! Tomorow is replace the fuel filters day. It is funny because the fuel filter hasn't so much as a tiny scratch on it and it is useless. BD cleans ! It is with great remorse that I will have to shut down production for the winter, but then it will give me time to get it together for next year. I am finding that my one good WVO supplier isn't able to keep up with me so that will be on the list of things to do too. The organic farmer today asked if he should buy a biodiesel truck, so we all know where THAT is going huh ? I make the fuel, he uses
RE: [Biofuel] Cold Weather Processing
I did graduate from college with a BA in Chemistry and I did do my senior thesis research on biodiesel. I didn't get anywhere near what I wanted to get accomplished with my project since the school I went to had virtually no working instruments to test with. I started with the straight forward biodiesel reaction with methanol and vegetable oil with NaOH catalyst and then tried a couple variations with ethanol. I also tried a couple ether-alcohols 1-methoxy-2-ethanol and 2 methoxy-ethanol. In those reactions, the glycerine combined with the alcohol instead of the fatty acid, and I was left with soap as the other product. It seemed that the reaction was temperature dependent as when the temperature for those 2 reactions was above 70 degrees celsius, there was definite glycerine present as the color of the reaction mix became a dark amber, but as the temperature dropped in the deparation vessel the brown color disappeared and became a milky cloudy color. Now, the only instrument available to me in the lab was NMR which wasn't very helpful to me other than to tell me qualitatively what I had, but not the purity. I was hoping to do some HPLC tests to see what kind of reaction % I was getting. I also tried using isopropanol which didn't work with the NaOH or KOH. I reacted Na metal with the isopropanol (I was using 99.5% pure and not rubbing alcohol) and a precipitate formed since the Na metal did not react vigorously enough before the oxygen in the air reacted to form NaOH. I tried potassium metal which reacted readily with the alcohol and using the potassium isopropoxide in isopropanol solution I had created as a catalyst, I was able to get a reaction just as in the complex ether-alcohols but the end result was similar... when the temperature dropped to room temperature in the separation vessel, the glycerine disappeared and I ended up with an unseparated product. I found also that using sodium metal (reacting on a mole-to-mole basis) with ethanol to get the same sodium concentration as with lye and this was the most effective route for me overall. There was no problem with separation and since there was no water produced in the reaction (the byproduct would be a sodium salt of glycerine) there was no emulsion when washing as I had experienced in the other tests. I don't know how feasible it would be to use sodium metal though, since it is highly reactive with water. I didn't have the time to try more complex tests than these, and was thoroughly disappointed that I couldn't do more instrumental analysis to find the purity of the product I produced. I should also note that you can purchase sodium ethoxide or sodium methoxide in salt form as well. I wish I knew where I kept the paper I found on the subject but there was a university study that showed that the use of sodium methoxide or sodium ethoxide was superior when working with pure ethanol, but that potassium ethoxide and methoxide did not yield a good separation... this I don't know why. Like I said, there was much more I wish I could have done, and I wish I could get in to the U of Idaho to work on biodiesel as a graduate student, but since they only accept 10 graduates (not all from the US of course) and I could have used a few extra points on my GPA, I'm not going to bother applying. Right now I am working a job that has nothing to do with what I want to do, but hopefully after I put in a couple years, I can get a better idea of what I want to do with my life. Regards, Jeff Original Message Follows From: Keith Addison [EMAIL PROTECTED] Reply-To: [EMAIL PROTECTED] To: [EMAIL PROTECTED] Subject: RE: [Biofuel] Cold Weather Processing Date: Sun, 10 Oct 2004 22:18:13 +0900 Hello Jeff I'm wondering if since water present in small amounts can impede the biodiesel reaction, if adding the water before removing as much glycerine as possible be a cause for some of the problems with separation and emulsions since there could be some extraneous reactions or possible reverse reactions going on in the mix? Have a look at this: http://infoarchive.net/sgroup/BIOFUEL/34062/ This is the glycerine wash step from Optimization of a Batch Type Ethyl Ester Process by the University of Idaho: http://journeytoforever.org/biofuel_library/ethyl_esters.html Ethyl Ester Process Also, in my experience, if you can get ahold of sodium methoxide or ethoxide (or if you can make it yourself using sodium metal reacted with ethanol or methanol) gives a much better separation of the biodiesel from the glycerine and the glycerine is much thicker. I would suggest that if you have trouble with separation, perhaps replacing as little as 25% of the NaOH or KOH used with the ethoxide salt (on a molar basis) and seeing how that works for you - adding more or less by trial and error until you get a satisfactory result. Also, using sodium ethoxide as a catalyst makes the use of ethanol
[Biofuel] Cold Weather Processing
G'day; Well, I have come across another part of the learning curve. My processor/wash tank combo resides in a non-winterized pump house and the last two times I have processed a batch of BD (80liters each) I had a problem with saponification/emulsion and I believe I have it figured out. As a side note, this probably would not have happend with KOH, but I am using NaOH at the moment. The temps here have gone down at night quite a bit of late and this is the time that the settling is being done. The last two times I had to heat the plumbing at the exit point of the reator in order to get the glycerine to flow, at the same time turning on the reactor's heat for about 30-45 minutes, as the glycerine had hardened in the plumbing as well as inside the reactor. Once the glycerine begins flowing it does so very well, HOWEVER it does not all come out as there is still some that gets melted while the hot BD is being transfered to the wash tank as witnessed by a sharp darkening of the colour in the sight tube as it comes out. I immediately stop the pump and drain the remainder out the glycerine drain at the bottom, but not before some of it has blended with the BD being transfered and this results in a layer of creamed chicken soup that won't break. The fuel is good, as the shake test proves, athough there is glycerine being mixed with the BD, not good. Solution? Re-heat the lot and pump mix again when hot and let setlle a few hours and drain, let settle some more and drain again until the volume approaches what would normally come out the glycerine drain when the weather is warm. Alternative solution? Send the lot, immediately after initial processing, into a seperate settling tank that has been set up using the standpipe design (metal tank with bungs downward), let settle and then drain out the BD FIRST via the standpipe and pumped to the wash tank, and then flip on the welded immersion heater that has been inserted near the floor of the secondary settling tank thereby heating the glycerine layer and making it flow easier. A visual over the edge will tell if the whole glycerine layer got drained or not and this way NO glycerine is getting in the BD. Better system yet? Use potassium hydroxide and don't worry about theabove time-consuming PITA (Pain In The Anatomy). As still somewhat of a beginner at this BD making stuff I have a whack of NaOH that I got from a chem supply house that now has to be used, although once I have thorougly pefected using my system and understanding it's ups and downs to where I ma comfortable with it's nuances I will be looking into KOH as a catalyst. That will be for the next season, as this one winds down due to cold and I don't have the with all to properly insulate the pump house, although I will be using the off-season to do that as well as set up the secondary settling tank in preparation for a full and rewarding production season next year. The off-season time will also be used to stock up on things like, methanol and WVO (it's pretty good stuff I get from the Chinese Restaurant and I want to get ahead of it for next year), and insulating the pump house which will allow me to get going earlier than if I only wait for it to be warm enough in the Spring. Ordering some WintronXC30 is also on the list for early Spring use and also for next winters' BD experience. It is too bad too as the Benz REALLY likes running on B100, and it iwll do so once weather and the ability to process permits. Who knows, maybe it will be sooner rather than later, but one thing certain, I will be working at it. Luc ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: [Biofuel] Cold Weather Processing
G'day; Well, I have come across another part of the learning curve. I was looking at some of your earlier posts, very interesting to chart your progress in the last six months or so. The learning curve is a bit like completion in the process, it never quite gets there, and the curve never flattens either, but you're not rock-climbing anymore or scaling overhangs, just a gentle incline now. Someone said learning how to make biodiesel is about as difficult as learning gardening or how to brew your own beer, which is probably about right. It's easy, but you don't ever stop learning either. Like life, eh? My processor/wash tank combo resides in a non-winterized pump house and the last two times I have processed a batch of BD (80liters each) I had a problem with saponification/emulsion and I believe I have it figured out. As a side note, this probably would not have happend with KOH, but I am using NaOH at the moment. The temps here have gone down at night quite a bit of late and this is the time that the settling is being done. The last two times I had to heat the plumbing at the exit point of the reator in order to get the glycerine to flow, at the same time turning on the reactor's heat for about 30-45 minutes, as the glycerine had hardened in the plumbing as well as inside the reactor. Once the glycerine begins flowing it does so very well, HOWEVER it does not all come out as there is still some that gets melted while the hot BD is being transfered to the wash tank as witnessed by a sharp darkening of the colour in the sight tube as it comes out. I immediately stop the pump and drain the remainder out the glycerine drain at the bottom, but not before some of it has blended with the BD being transfered and this results in a layer of creamed chicken soup that won't break. The fuel is good, as the shake test proves, athough there is glycerine being mixed with the BD, not good. Solution? Re-heat the lot and pump mix again when hot and let setlle a few hours and drain, let settle some more and drain again until the volume approaches what would normally come out the glycerine drain when the weather is warm. :-( Alternative solution? Send the lot, immediately after initial processing, into a seperate settling tank that has been set up using the standpipe design (metal tank with bungs downward), let settle and then drain out the BD FIRST via the standpipe and pumped to the wash tank, and then flip on the welded immersion heater that has been inserted near the floor of the secondary settling tank thereby heating the glycerine layer and making it flow easier. A visual over the edge will tell if the whole glycerine layer got drained or not and this way NO glycerine is getting in the BD. That's how we do it with the 90-litre processor. The processor and holding tank both have a T-section and two valves fitted to the bottom drain, one valve for draining off the glycerine by-product, the other for transferring the biodiesel to the washing tanks via the pump. We use a couple of short lengths of PVC waterpipe narrowed at one end to fit inside the outlet drains. The length (height) of the pipes is calculated to be higher than the depth of by-product in the bottom of the tank after settling. This stand-pipe means the biodiesel can be pumped out to the washing tanks without getting any by-product in it. Later we remove the stand-pipe and drain off the by-product. The drained glyc comes with a bit of biodiesel left on top, after it's settled again the biodiesel is easily poured off into whichever wash tank isn't being used, ready for the next wash. A couple of times, before I started using the standpipes, I did manage to get some glyc by-product mixed in with the biodiesel, but it wasn't a problem. As soon as it was all transferred to the wash tank I chucked a bucketful of water on top of it, quite roughly, and left it to settle for an hour, which seemed to remove the glyc, or anyway there weren't any washing problems after that. It was quite a lot of glyc, not just a few cc. Sorry Luc, I've lost track - do you have your secondary settling tank set up already or is it the intention? Better system yet? Use potassium hydroxide and don't worry about theabove time-consuming PITA (Pain In The Anatomy). Yes. Your winter temps are lower than ours are, but it does hit -15 deg C here (5 deg F) here, and using KOH the glyc has never solidified. Anyway, did this complicate your results with the sprinkler wash system? As still somewhat of a beginner at this BD making stuff I have a whack of NaOH that I got from a chem supply house that now has to be used, although once I have thorougly pefected using my system and understanding it's ups and downs to where I ma comfortable with it's nuances I will be looking into KOH as a catalyst. That will be for the next season, as this one winds down due to cold and I don't have the with all to properly
