Todd, Just as predicted: The mono-, di- & triglycerids made another yucky emulsion after washing the "crystal clear" settled "biodiesel". Just to confirm once again the disadvantages of including water in the reaction. I thought water only caused soaps. Putting pieces together, now it«s clear that water also prevent the completion of the reaction (forming soaps consumes sodium necessary for the transesterification)
Christian ----- Original Message ----- From: "Appal Energy" <[EMAIL PROTECTED]> To: <biofuel@yahoogroups.com> Sent: Friday, June 28, 2002 1:24 PM Subject: Re: [biofuel] salty water > Christian, > > Yup. I'm sure. Been that. Done there... in a 350 gallon batch no > less. Ten gallons of what couldn't be salted out and didn't break > on its own over time are still sitting in a jug one year later. > > If you get as high a volume of emulsion as you stated, it's an > incomplete reaction and the presence of mono- and di-glycerides > that caused the enormity of it, not the soap, as most of the soap > drops with the glycerin. > > Try this for starters. Take the fluid whose emulsion was broken > with the salting out and submit it to another wash. It's a safe > bet that it will emulsify radically all over again. (You might > also set aside a bit and submit it to a second transeserification > to see how much glycerin drops out.) > > If you decant the fluid off the top that didn't emulsify and > submit it to another wash, that might be a fair indicator as to > how much of your incomplete reaction (mono- and di-glycerides) > went into the emulsified layer, but would depend greatly upon the > level of agitation during the initial wash. The decanted layer > might emulsify every bit as severely as the original washed > batch. > > I haven't seen any charts that can predict how heavy an emulsion > will occur in the presence of "x" mono- or di-glycerides. But I'm > sure there are some rules of thumb. A quick look at the back of a > mayonaise jar or many other food products lends one to believe > that it takes very little to achieve an extensive result. > > A few percent could be all it takes. That same few percent > wouldn't even be noticeable in a test for viscosity using > anything but the most advanced and electronically calibrated > equipment. > > A good number of persons would argue over this, but I'd say pack > the viscometer up in it's case and rely upon your wash > characteristics as indicators of a complete reaction, in absence > of a GC and or in a backyard environment. > > One other thing, relative to the quality of the salted out fluid. > I used to point out to our chemist that "Hell...diesel engines > will run on straight veg oil!" whenever he pointed out that we > were still none too sure about the quality of our fuel. Then I > tried running some of the salted out batch mentioned above. > > Sputter...sputter....gasp!!....hiss..! wheeze...!!!! Pure murder > for the first 3 minutes on a cold start at 50*F. When the "fuel" > was exhausted it was replaced with biodiesel from a less > troublesome batch. The car turned around and slapped a big wet > one on us in thanks for treating it better. > > Todd Swearingen > > ----- Original Message ----- > From: Christian <[EMAIL PROTECTED]> > To: <biofuel@yahoogroups.com> > Sent: Friday, June 28, 2002 8:52 AM > Subject: Re: [biofuel] salty water > > > Dear Todd, > > Is that so? The mini batch I experimented on seemed to show a > good > conversion. Of course I did not run it through a gas > chromatograph, but the > BD seemed OK (not emulsified or mixed with oils and mono- & di- > glycerids). > The mixture of EtOH and MeOH I used resulted in 98% alcohol, and > I suppose > 2% water is just in the limit of acceptance for a > transesterification > reaction (don«t know... I assume this out of experience). Anyhow, > the > ammount of water I had was too much and everything emulsified in > a thick > white foam. But the NaCl and a light rewash with the salty water > reduced > everything from the former "20% BD, 70% foam, 10% water" to a > "50% BD, 5% > foam, 45% water"... or something like that. and the BD is now > settling its > turbidity and taking the typical transparent pale golden colour. > Viscosity > seems OK (inidcating absence of glycerides?).... Are you sure > it«s such an > incomplete reaction? > > Thanks again for your help, > > Christian > ----- Original Message ----- > From: "Appal Energy" <[EMAIL PROTECTED]> > To: <biofuel@yahoogroups.com> > Sent: Thursday, June 27, 2002 12:15 AM > Subject: Re: [biofuel] salty water > > > > Christian, > > > > I believe the emulsion breaking process you are referring to is > > called "salting out" in chemistry vernacular. > > > > Unfortunately, it's not biodiesel that you are salting out. > > Rather, it's mono- and di-glycerides from an incomplete > reaction. > > > > Anytime that you have that much of an emulsion problem, you > can't > > bet your burrow and its saddle that's the problem. > > > > If you take the salted-out, recovered "fuel" and run it through > > the transesterification process again, you will find that a > good > > bit more glycerin drops out. > > > > You will also find that if you try and run the salted-out, > > recovered "fuel" in an engine, the exhaust will be considerably > > denser white than when running completed biodiesel. > > > > Another minor problem with using NaCl in such a manner, > > especially when running larger batches, is the toxicity of > salt. > > Such a practice completely prevents the disposal of grey water > in > > an irrigation type application. It's okay in small experimental > > quantities. But production levels for personal use or greater > > begin to incur problems. > > > > Best solution? Get the transesterification process down where > you > > know the reaction has completed. Might take some doing when > > working with a variable such as ethanol. > > > > Todd Swearingen > > > > ----- Original Message ----- > > From: Christian <[EMAIL PROTECTED]> > > To: <biofuel@yahoogroups.com> > > Sent: Wednesday, June 26, 2002 11:01 PM > > Subject: [biofuel] salty water > > > > > > Hi all. > > > > Can«t remember if this issue was discussed at some point but > it«s > > worth refreshing it: > > > > The first washing stages could use some salty water to avoid > > emulsification problems. > > > > Saturated ordinary salt (NaCl) solutions are useful as many > > substances which are soluble in water are insoluble or > partially > > soluble in salty water. In our case, BD production presents a > > minor problem with soap formation and emulsification problems, > > specially in the first washing stages and if water is present. > > > > I made a test with 25% of 96¼ Ethanol + 75% of 98,8% Methanol > > some time ago. The BD came out crystal clear after settling, > but > > the first washing stage left a messy emulsion that was stabel > for > > over three weeks. I finally got bored of the "wait and see" > > method and tried to break the emulsion with a fresh salty water > > solution. I managed to recover most of the emulsified BD. > > > > Please consider using salty water in your first washes, > specially > > if you think you might have problems with soap formation > (usually > > due to presence of water or high FFA content, which shows up as > a > > high value in the titration, probably above 2 or 3 ml (of > 0,025M > > NaOH, or 1g lye/ lt of water solution). > > > > The salt should wash away with the aqueous phase, and the > second > > and third washes will handle that OK. > > > > Best wishes, > > > > Christian > > > > > > [Non-text portions of this message have been removed] > > > > > > Biofuel at Journey to Forever: > > http://journeytoforever.org/biofuel.html > > > > Biofuels list archives: > > http://archive.nnytech.net/ > > > > Please do NOT send "unsubscribe" messages to the list > > address. > > To unsubscribe, send an email to: > > [EMAIL PROTECTED] > > > > Your use of Yahoo! Groups is subject to the Yahoo! 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