Re: [Biofuel] BD process question
Hello Joe Hi Keith See my answers below; Keith Addison wrote: Hello Joe Hello, I have a question about biodiesel processing I hope someone can help me with; I read the excellent info on the journey to forever site and checked the archives about washing etc. I am interested in using mechanical agitation to speed up the process of washing but I wonder if I am being too impatient or something. Did you see this post? http://www.mail-archive.com/biofuel@sustainablelists.org/msg37937.html Re: [biofuel] Circulation with pump washing. I just read it. Thanks. I don't think hot biodiesel fumes are very good for you. The smell is certainly more aromatic. This is the first I have heard of this. I thought I read on JtoF that BD is completely non toxic. It is, but does that also mean the fumes from heating it to a high temperature are harmless? I don't know. I've seen some people claiming it's harmful but without any details and I've never been able to find any real info on it. I'm afraid I'm a dumbo when it comes to vacuum, I don't know what that means. Did you let the glycerin by-product settle and separate it before distilling off the excess methanol? If you did it straight after the reaction you probably sent the reaction into reverse, converting soaps back into FFAs, which dissolve in the biodiesel and can't be washed out (and are not good for your motor). Either way, I doubt you'd succeed in removing all the excess methanol by distillation, most perhaps but not all. If you distilled it off with the by-product still in the reactor there'd still be quite a lot left in the by-product - without using vacuum you'd need to finish at a temperature of about 150 deg C to get it all, or nearly all. Anyway if you washed it thoroughly there won't be any methanol left. I let the glycerine settle overnight and then I turned the rercirc pump back on and mixed it all up while heating to 55 deg C. Then I used vacuum until the distillate stopped and then vented and allowed it to separate again. I doubt you got 100% of the methanol out that way, and you do risk reversing the reaction. I drained off the glycerin and added hot tap water ( I used deionized water in my test batches that is one difference) and recirculated for about an hour. After washing I would let it separate for two hours and then drain the water and repeat. I used 3 wash cycles. The last wash water came out almost clear. Try another wash cycle. Washing it in the processor runs the risk of contamination with residual by-product. See how it goes, you might have this problem later and need a separate wash-tank. Does the cloudiness indicate that the reaction was not correct (excess caustic?) If it's really persistent it might do. But you haven't told us very much about what you did, titration etc. - how did you measure the pH? Did you measure the pH of the final batch of wash water? It should be the same as your tap water. There are quite a lot of variables in transferring a process from a one-litre test batch to a bigger processor. You might need to experiment with agitation times. What's the volume of your reactor, only five gallons? I used phenolthalien (a few drops) in 4 ml oil mixed with 40 ml IPA. I stopeed when the color lasted 10 seconds. I don't have my lab book with me at work here but I think it came out around 3.5 ml of 0.1 % KOH soln per ml. Following the recommendations regarding the assay of my KOH I ended up deciding on 10.6 g KOH per liter of oil for my process. I did get a good clean split this way. Sounds good. I haven't tried reducing the concentration of caustic yet. I haven't measured the was water ph. I will do this. Yes my batch reactor is pitifully small. It is a 36 liter hot water tank. Since I walk to work year round my fuel needs are relatively low and my Golf TDI sips fuel rather than being a big gulper so I opted to build a small system that fits in my basement. I don't think that's pitiful, Joe, I think it's admirable, especially in view of your previous message about the footprints we make on the face of this fair planet. We fuelled our Toyota TownAce for nearly a year with a 20-litre processor, this one: http://journeytoforever.org/biodiesel_processor5.html Simple 5-gallon processor The TownAce isn't nearly as economical as your Golf, and we also fuelled a few tractors and provided biodiesel for demos and for people coming to our seminars and so on. Now we make 60-litre batches but we still use the 5-gallon processor. Lots of people have copied it. I do wonder about people, especially in the US, who just seem to be ordinary folks, not farmers or businesses with fleets or whatever, but they say a 200-litre processor isn't enough for them. I use forced exhaust to take any fumes away from the methoxide mixing and the vacuum pump exhaust when it is running. So far it works ok except I guess I am pushing the process just a
[Biofuel] BD process question
Hello, I have a question about biodiesel processing I hope someone can help me with; I read the excellent info on the journey to forever site and checked the archives about washing etc. I am interested in using mechanical agitation to speed up the process of washing but I wonder if I am being too impatient or something. Some background on what I am doing I have been using the single stage process so far. I started to learn with virgin canola oil and then went to waste canola oil from a local pub. In every case I have done my titrations carefully using a good quality burette and stock KOH solution carefully mixed using a laboratory grade electronic scale and DI water. When I did the 1 liter test batches I got a clean split with only 2 layers and after 4 washes with acetic acid on the first one I have ended up with BD that is cloudy. After heating the BD for drying it became spectrally clear and remained that way after cooling. I had given an extended waiting time of more than a week to see if it would clarify on it's own but this did not happen. After the clarification by heating I took it down to the freezing point and it remained clear after thawing. Then I did my first 5 gallon batch in a water heater. My reractor is a vacuum type and I use a circulation pump for mixing and washing etc. Again I obtained a good clear split but this time the BD clarified after heating (began to clear at about 50 deg. C. and I heated it to 135 deg C.) and I was shocked to see it cloudy the following day after it cooled. I reheated again this time to 170 deg. C. and it was better after cooling but not near as clear as the other 1 liter test batches. So questions: What is it exactly that causes the cloudiness? Is it water content? I notice the BD from the test batches after all is done has a smell similar to oil based paint or linseed oil but had a much sweeter aromatic smell while it was being heated. The large batch more so. Is this due to residual methanol (which I thought I completely removed after the reaction using vacuum distillation at 55 deg C and 25 in Hg)? Does the cloudiness indicate that the reaction was not correct (excess caustic?) I didn't have a problem with soaps. Any recommendations? Thanks in advance for any help you can offer Joe ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] BD process question
Hello Joe. The cloudiness is most likely caused by water or water soluble substances. A simple way of approaching your problem is to put your mini batch into water about 60-65oC, and let it stay there for a few hours. If it becomes clear, let it stay there for some additional time. If it does not become clear, try washing it again several times with water only and repeat the hot water procedure. Jan Warnqvist AGERATEC AB [EMAIL PROTECTED] + 46 554 201 89 +46 70 499 38 45 - Original Message - From: Joe Street [EMAIL PROTECTED] To: Biofuel@sustainablelists.org Sent: Tuesday, June 28, 2005 3:26 PM Subject: [Biofuel] BD process question Hello, I have a question about biodiesel processing I hope someone can help me with; I read the excellent info on the journey to forever site and checked the archives about washing etc. I am interested in using mechanical agitation to speed up the process of washing but I wonder if I am being too impatient or something. Some background on what I am doing I have been using the single stage process so far. I started to learn with virgin canola oil and then went to waste canola oil from a local pub. In every case I have done my titrations carefully using a good quality burette and stock KOH solution carefully mixed using a laboratory grade electronic scale and DI water. When I did the 1 liter test batches I got a clean split with only 2 layers and after 4 washes with acetic acid on the first one I have ended up with BD that is cloudy. After heating the BD for drying it became spectrally clear and remained that way after cooling. I had given an extended waiting time of more than a week to see if it would clarify on it's own but this did not happen. After the clarification by heating I took it down to the freezing point and it remained clear after thawing. Then I did my first 5 gallon batch in a water heater. My reractor is a vacuum type and I use a circulation pump for mixing and washing etc. Again I obtained a good clear split but this time the BD clarified after heating (began to clear at about 50 deg. C. and I heated it to 135 deg C.) and I was shocked to see it cloudy the following day after it cooled. I reheated again this time to 170 deg. C. and it was better after cooling but not near as clear as the other 1 liter test batches. So questions: What is it exactly that causes the cloudiness? Is it water content? I notice the BD from the test batches after all is done has a smell similar to oil based paint or linseed oil but had a much sweeter aromatic smell while it was being heated. The large batch more so. Is this due to residual methanol (which I thought I completely removed after the reaction using vacuum distillation at 55 deg C and 25 in Hg)? Does the cloudiness indicate that the reaction was not correct (excess caustic?) I didn't have a problem with soaps. Any recommendations? Thanks in advance for any help you can offer Joe ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] BD process question
--- Joe Street [EMAIL PROTECTED] wrote: Hello, I have a question about biodiesel processing I hope someone can help me with; I read the excellent info on the journey to forever site and checked the archives about washing etc. I am interested in using mechanical agitation to speed up the process of washing but I wonder if I am being too impatient or something. Some background on what I am doing I have been using the single stage process so far. I started to learn with virgin canola oil and then went to waste canola oil from a local pub. In every case I have done my titrations carefully using a good quality burette and stock KOH solution carefully mixed using a laboratory grade electronic scale and DI water. When I did the 1 liter test batches I got a clean split with only 2 layers and after 4 washes with acetic acid on the first one I have ended up with BD that is cloudy. After heating the BD for drying it became spectrally clear and remained that way after cooling. I had given an extended waiting time of more than a week to see if it would clarify on it's own but this did not happen. After the clarification by heating I took it down to the freezing point and it remained clear after thawing. Then I did my first 5 gallon batch in a water heater. My reractor is a vacuum type and I use a circulation pump for mixing and washing etc. Again I obtained a good clear split but this time the BD clarified after heating (began to clear at about 50 deg. C. and I heated it to 135 deg C.) and I was shocked to see it cloudy the following day after it cooled. I reheated again this time to 170 deg. C. and it was better after cooling but not near as clear as the other 1 liter test batches. So questions: What is it exactly that causes the cloudiness? Is it water content? I notice the BD from the test batches after all is done has a smell similar to oil based paint or linseed oil but had a much sweeter aromatic smell while it was being heated. The large batch more so. Is this due to residual methanol (which I thought I completely removed after the reaction using vacuum distillation at 55 deg C and 25 in Hg)? Does the cloudiness indicate that the reaction was not correct (excess caustic?) I didn't have a problem with soaps. Any recommendations? Thanks in advance for any help you can offer Joe ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/ biodiesel is hygroscopic. on cooling it absorbs water. if yopu want it to be clear try puttng an air tight lid on it. fox ___ Yahoo! Messenger - NEW crystal clear PC to PC calling worldwide with voicemail http://uk.messenger.yahoo.com ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] BD process question
Hello Joe Hello, I have a question about biodiesel processing I hope someone can help me with; I read the excellent info on the journey to forever site and checked the archives about washing etc. I am interested in using mechanical agitation to speed up the process of washing but I wonder if I am being too impatient or something. Did you see this post? http://www.mail-archive.com/biofuel@sustainablelists.org/msg37937.html Re: [biofuel] Circulation with pump washing. Some background on what I am doing I have been using the single stage process so far. I started to learn with virgin canola oil and then went to waste canola oil from a local pub. In every case I have done my titrations carefully using a good quality burette and stock KOH solution carefully mixed using a laboratory grade electronic scale and DI water. When I did the 1 liter test batches I got a clean split with only 2 layers and after 4 washes with acetic acid on the first one I have ended up with BD that is cloudy. After heating the BD for drying it became spectrally clear and remained that way after cooling. I had given an extended waiting time of more than a week to see if it would clarify on it's own but this did not happen. It should have though, especially in mid-summer. After the clarification by heating I took it down to the freezing point and it remained clear after thawing. Then I did my first 5 gallon batch in a water heater. My reractor is a vacuum type and I use a circulation pump for mixing and washing etc. Again I obtained a good clear split but this time the BD clarified after heating (began to clear at about 50 deg. C. It should begin to clear at about 30 deg C, or less. and I heated it to 135 deg C.) Ouch! Too much heat! No need. and I was shocked to see it cloudy the following day after it cooled. I reheated again this time to 170 deg. C. and it was better after cooling but not near as clear as the other 1 liter test batches. So questions: What is it exactly that causes the cloudiness? Is it water content? Yes. It's almost always hazy after washing and needs a bit of time to settle. Leave it in the sun for a while. Or heat it to 50 deg C and let it cool in a vented container. This causes the microdroplets of water suspended in the fuel to evaporate off. You can do that twice if you need to, but you shouldn't need to. If that doesn't work and it goes hazy again you probably haven't washed it enough. Once the washed fuel is clear at room temperatures it is considered to be dry, although there will always be some water dissolved in it, not problem, unlike suspended water, which would be a problem. I notice the BD from the test batches after all is done has a smell similar to oil based paint or linseed oil but had a much sweeter aromatic smell while it was being heated. I don't think hot biodiesel fumes are very good for you. The smell is certainly more aromatic. The large batch more so. Is this due to residual methanol (which I thought I completely removed after the reaction using vacuum distillation at 55 deg C and 25 in Hg)? I'm afraid I'm a dumbo when it comes to vacuum, I don't know what that means. Did you let the glycerin by-product settle and separate it before distilling off the excess methanol? If you did it straight after the reaction you probably sent the reaction into reverse, converting soaps back into FFAs, which dissolve in the biodiesel and can't be washed out (and are not good for your motor). Either way, I doubt you'd succeed in removing all the excess methanol by distillation, most perhaps but not all. If you distilled it off with the by-product still in the reactor there'd still be quite a lot left in the by-product - without using vacuum you'd need to finish at a temperature of about 150 deg C to get it all, or nearly all. Anyway if you washed it thoroughly there won't be any methanol left. Does the cloudiness indicate that the reaction was not correct (excess caustic?) If it's really persistent it might do. But you haven't told us very much about what you did, titration etc. - how did you measure the pH? Did you measure the pH of the final batch of wash water? It should be the same as your tap water. There are quite a lot of variables in transferring a process from a one-litre test batch to a bigger processor. You might need to experiment with agitation times. What's the volume of your reactor, only five gallons? I didn't have a problem with soaps. Any recommendations? I don't think you have any major problems, you're doing well! Keep going, refine your methods and techniques through practice, keep doing comparative checks with the quality tests here: http://journeytoforever.org/biodiesel_vehicle.html#quality It's just a matter of time until you're making high-quality biodiesel that washes easily and dries easily too. Best wishes Keith Thanks in advance for any help you can offer Joe
Re: [Biofuel] BD process question
Hi Keith See my answers below; Keith Addison wrote: Hello Joe Hello, I have a question about biodiesel processing I hope someone can help me with; I read the excellent info on the journey to forever site and checked the archives about washing etc. I am interested in using mechanical agitation to speed up the process of washing but I wonder if I am being too impatient or something. Did you see this post? http://www.mail-archive.com/biofuel@sustainablelists.org/msg37937.html Re: [biofuel] Circulation with pump washing. I just read it. Thanks. I don't think hot biodiesel fumes are very good for you. The smell is certainly more aromatic. This is the first I have heard of this. I thought I read on JtoF that BD is completely non toxic. I'm afraid I'm a dumbo when it comes to vacuum, I don't know what that means. Did you let the glycerin by-product settle and separate it before distilling off the excess methanol? If you did it straight after the reaction you probably sent the reaction into reverse, converting soaps back into FFAs, which dissolve in the biodiesel and can't be washed out (and are not good for your motor). Either way, I doubt you'd succeed in removing all the excess methanol by distillation, most perhaps but not all. If you distilled it off with the by-product still in the reactor there'd still be quite a lot left in the by-product - without using vacuum you'd need to finish at a temperature of about 150 deg C to get it all, or nearly all. Anyway if you washed it thoroughly there won't be any methanol left. I let the glycerine settle overnight and then I turned the rercirc pump back on and mixed it all up while heating to 55 deg C. Then I used vacuum until the distillate stopped and then vented and allowed it to separate again. I drained off the glycerin and added hot tap water ( I used deionized water in my test batches that is one difference) and recirculated for about an hour. After washing I would let it separate for two hours and then drain the water and repeat. I used 3 wash cycles. The last wash water came out almost clear. Does the cloudiness indicate that the reaction was not correct (excess caustic?) If it's really persistent it might do. But you haven't told us very much about what you did, titration etc. - how did you measure the pH? Did you measure the pH of the final batch of wash water? It should be the same as your tap water. There are quite a lot of variables in transferring a process from a one-litre test batch to a bigger processor. You might need to experiment with agitation times. What's the volume of your reactor, only five gallons? I used phenolthalien (a few drops) in 4 ml oil mixed with 40 ml IPA. I stopeed when the color lasted 10 seconds. I don't have my lab book with me at work here but I think it came out around 3.5 ml of 0.1 % KOH soln per ml. Following the recommendations regarding the assay of my KOH I ended up deciding on 10.6 g KOH per liter of oil for my process. I did get a good clean split this way. I haven't tried reducing the concentration of caustic yet. I haven't measured the was water ph. I will do this. Yes my batch reactor is pitifully small. It is a 36 liter hot water tank. Since I walk to work year round my fuel needs are relatively low and my Golf TDI sips fuel rather than being a big gulper so I opted to build a small system that fits in my basement. I use forced exhaust to take any fumes away from the methoxide mixing and the vacuum pump exhaust when it is running. So far it works ok except I guess I am pushing the process just a tad with regard to the washing and drying. I'll give it more time next time and see if it improves. Thanks for your suggestions. Joe ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
