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New Methods #2. The Imisides Method

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  • #46
    Re: New Methods #2. The Imisides Method

    Originally posted by timorcoco View Post
    The most appealing aspect of this method is the promise of less soap made due to less water formation at
    meth and reaction stages .
    perhaps a soap test would be in order - by titration or water mix
    Have you done any checks Mark , and could you please explain further why you feel water wash of product is unsuitable.
    maybe this method + woodchip drywash could be the go . . . . . .
    The most appealing aspect of this method to me was the fact that it proceeds at room temperature. Although it produces less soap, the fact that it is utterly anhydrous is what is relevant, as soap is only a problem when there is water present to emulsify.

    Soap is certainly not a problem on its own. Guys that run SVO have no problem with FFAs in their fuel, and it's hard to see why the sodium or potassium salt of the FFA (soap) would be a problem. So no, I haven't tested for soap level, and see no reason why I would want to. Theoretically, the soap level would be a direct function of the FFA level, as this is the only source of soap in this method.

    The reason I'd recommend against water washing is that with the far higher level of KOH (which is regenerated in the transesterification process) you may saponify the methyl ester you've just made. I'm not an organic chemist so I can't speak with any authority on the kinetics or mechanism of this process - my gut feeling is that at RT it'd be minimal, but you never know.

    In any case, water washing is utterly unnecessary, regardless of what method you use.

    These things ar OK in your fuel:

    1. Methyl ester
    2. Unconverted WVO (unless there is enough of it to affect the viscosity)
    3. FFA
    4. soap

    These things are not OK in your fuel

    1. MeOH (will attack o-rings)
    2. KOH (will dissolve the alloy in your IP)
    3. Glycerol (will settle as a thick sludge in your fuel tank that will clog your fuel lines - ask me how I know that!!)

    Luckily, the last two of these are removed (fall into the glycerol) when you remove the first by evaporation

    One other comment - I'm a little curious to know where the soaps go in an anhydrous method like mine. Since there is no water to form micelles, it likely accumulates at the glycerol/biodiesel interface (such is the nature of surfactants) although depending on its HLB (hydrophilic lipophilic balance) it may actually partition into either phase.

    The only bloke that I (privately) released this method to is a chap named Murf - his silence on this thread is probably a fact that it's such a simple, foolproof method, he never needs to come looking for help.

    BTW, what's a woodchip drywash - sounds interesting.

    Comment


    • #47
      Re: New Methods #2. The Imisides Method

      Hi Mark,

      Originally posted by Dr Mark View Post
      Although it produces less soap, the fact that it is utterly anhydrous is what is relevant,
      Utterly anhydrous? That is not what you have said on pages 2 and 4.
      On page 2 you said; "I always felt that I'd never added enough lime to completely dehydrate the methoxide solution, but only enough to do the job...It doesn't need to fully dehydrate the methoxide solution. It just needs to pull the eq to the right to make enough MeO- to allow the rxn to proceed at RT"
      then on page 4, you said; "rather than having water present from both your WVO and methoxide solution, there would only be water from the WVO"
      Your process is far from being "Utterly anhydrous"

       
      Theoretically, the soap level would be a direct function of the FFA level, as this is the only source of soap in this method.
      You seem to be forgetting about the water that you say is still contained in your methanol/KOH mix and the WVO.


      I'm not an organic chemist so I can't speak with any authority on the kinetics or mechanism of this process.
      Yes, that has been clear for a long time.
      tillyfromparadise
      Senior Member
      Last edited by tillyfromparadise; 18 November 2011, 11:40 PM.

      Comment


      • #48
        Re: New Methods #2. The Imisides Method

        Dr Mark,

        'Utterly anhydrous' - That's a big claim and one I suspect you'd be hard pressed to substantiate.
        Particularly since you cannot tell us precisely how much CaO to use.
        It started out as 'two shovels' then you narrowed it slightly to:
        I used about twice as much (by sight) lime as I did KOH and that seemed to dehydrate the process enough to get enough methoxide in solution to get the reaction to proceed at RT.
        The link I posted here:

        Desiccant Chart Comparisons - SorbentSystems.com

        seems to suggest that we might need more than 3 times the amount of caustic, as the equilibrium capacity (H2O) of CaO is less than 30%, and this would need to be kept in suspension for several days to be fully effective because the adsorption rate is so slow.

        As I understand it, there are 3 primary sources of water in the biodiesel reaction:

        1. Created by dissolving the chosen caustic in MeOH
        2. Created by the soap making reaction of FFA with the chosen caustic
        3. Pre-existing suspended/dissolved moisture in the feedstock WVO

        Your process partially addresses source No.1 but does nothing to influence sources 2 and 3, so there will always be some water present.
        Can you contact your confidante 'Murf' and ask him to give us some specific details and first hand experience please?
        geewizztoo
        Senior Member
        Last edited by geewizztoo; 21 November 2011, 11:39 AM.

        Comment


        • #49
          Re: New Methods #2. The Imisides Method

          well there ya go, I haven't read all the posts yet but will go read them now

          over 3 years of making BIO and over 10,000ltrs in the last year and never had a problem

          I have kept an eye out over the years and can't believe no one had come up with this simple solution

          thanks Mark and I have never let this great method be know to anyone and would have never kept it up if it wasn't so easy

          quicklime has just become my main problem at $80 delivered for a 25kg bag (was $40/25kg for last three years) I am going to buy a 1 Tonne bag and vac seal it in 5kg bags (the amount I use for 55ltr of Methoxide)

          have just made 800ltrs in the last three weeks

          cheers Murf
          3 years of BD100 using the Dr Mark Imisides method, currently making 10,000lt/year

          1991 GQ Patrol 4.2 with DTS turbo

          Comment


          • #50
            Re: New Methods #2. The Imisides Method

            Hi Murf,
            10,000 litres of biodiesel a year is pretty impressive.
            I would be hard pressed to have done that in the last 4 years.
            After Mark mentioned your name I did have a read through all your posts and did not twig to the fact that you were making such huge quantities of biodiesel.
            With those quantities I imagine you have been very careful to document all the testing you performed and their results on each batch of biodiesel you produced.

            I am sure everyone would really like to see the testing you performed and the results.
            tillyfromparadise
            Senior Member
            Last edited by tillyfromparadise; 22 November 2011, 10:45 PM.

            Comment


            • #51
              Re: New Methods #2. The Imisides Method

              BTW, there is a bloke named Murf who used to be on this forum who's been making his bio with this method for a couple of years now. If he could be contacted he might have some comments

              hello

              reading reading reading

              cheers Murf
              3 years of BD100 using the Dr Mark Imisides method, currently making 10,000lt/year

              1991 GQ Patrol 4.2 with DTS turbo

              Comment


              • #52
                Re: New Methods #2. The Imisides Method

                Quicklime - It's not a DG, so there should be no special transport or storage considerations involved. When I bought it over the counter I think I paid $12 for a 20kg bag. From memory it was a 90% purity product, with most of the rest of it being MgO

                the Tamworth plant won't let me pick it up in a trailer, has to be on a truck with cages straps and tarps, awaiting transport notes and delivery price, Quicklime is $300/Tonne

                cheers Murf
                3 years of BD100 using the Dr Mark Imisides method, currently making 10,000lt/year

                1991 GQ Patrol 4.2 with DTS turbo

                Comment


                • #53
                  Re: New Methods #2. The Imisides Method

                  Originally posted by tillyfromparadise View Post
                  Hi Murf,

                  With those quantities I imagine you have been very careful to document all the testing you performed and their results on each batch of biodiesel you produced.

                  I am sure everyone would really like to see the testing you performed and the results.
                  mate I did all sorts of tests I could find at the time and gave Mark a heap of questions when I first began making Bio, to be honest I now don't do any testing of any sort other than a sniff test to see how much methanol is in the bubbling tank and a quick sight test in a class jar to see how clear it is before pumping to my 1300ltr storage tank

                  I use one of those 60ltr home brew drums to mix the methanol and Koh then the Quicklime, I do 55ltr batches at a time,
                  the valve is high enough on the home brew drum with a little back slant on the drum to decant the methoxide off the top of the settled CaO into 20lt containers (17ltrs as there is 2 ltrs left at level) this is then gravity fed into my processor

                  I live on a 120ac property and the lime is spread over the paddocks, yep it kills the grass at first if put on in one dump but soon all is good again

                  this is such a KISS system and any monkey can do it as I am proof over the years (don't tell anyone as I will have a fight to keep my oil supplies )

                  I have no idea of what titration I have as I have never tested it ever??? some really ugly looking oil/fat will give me more by-product but who cares, I just churn it out and use it

                  I do heat the oil to around 50deg C I think, haven't tested it for a couple of years, I time the heater and put my hand on the tank to see if it is too hot.

                  the only problem I have had is the mates 80 series 1HZ injector pump rattles like a marble in a shaken tin can, he had the pump fixed for $1300 and it still did the same thing haha, a pusher pump fixed that and has since put 5000ltrs or so through it

                  oh and my GQ didn't like a sub zero morning running frytoll LARD once lucky I had power and a fan heater

                  in short you don't have to be a biochemist to do it, it is very financially rewarding, only takes up a couple of hours of my time a week and most importantly allows me to do things that I could not afford before I started making BIO (thanks again Mark )

                  on the negative its messy and there are literally hundreds of drums sitting around the place, I have made several oops by leaving valves open and filling the dam with a couple of hundred ltrs of BIO and WVO a couple of times (never walk away or get distracted when draining by-product or water from storage tanks)

                  so tied and have a screaming headache so if what I said don't make sense then there's ya answer haha

                  cheers Murf
                  3 years of BD100 using the Dr Mark Imisides method, currently making 10,000lt/year

                  1991 GQ Patrol 4.2 with DTS turbo

                  Comment


                  • #54
                    Re: New Methods #2. The Imisides Method

                    Hi Murf,
                    Thank you for your reply.
                    Can you be more specific as to what tests you have performed.
                    Did you ever do a 3/27 test?
                    What size batches of biodiesel do you make?

                    What formula do you use to make biodiesel?
                    In particular how much methanol and how much KOH and CaO do you use for each litre of oil reacted?
                    For instance, while Mark's instructions are a bit vague. as close as I can make out, Mark seems to recommend using 150ml methanol, 15g KOH and 30g CaO for each litre of WVO being reacted. That would work out to 15 litres of methanol per 100 litre of WVO being reacted.
                    tillyfromparadise
                    Senior Member
                    Last edited by tillyfromparadise; 23 November 2011, 09:07 AM.

                    Comment


                    • #55
                      Re: New Methods #2. The Imisides Method

                      A book, Practical Organic Chemistry written by Vogel gives a laboratory procedure for drying 95% ethanol to 99.5% dry ethanol. It uses Calcium Oxide to pull out the water leaving almost anhydrous ethyl alcohol. 500 grams of Calcium Oxide is put into 2 litres of 95% ethanol, then 6 hour reflux, then sits overnight in a sealed flask, then the 99.5% dried ethanol is distilled off. In the book next is a procedure for making super dry ethanol. The book says methanol may also be dried using Calcium Oxide. I think it doesn't take out all the water, but it gets most of it out.

                      Comment


                      • #56
                        Re: New Methods #2. The Imisides Method

                        Thanks Murf for joining this interesting discussion.

                        Can you tell us your recipe and procedure? ie. specific quantities, mix ratios, times, etc?

                        I'm particularly interested in your methoxide mixture, I assume you put the KOH in first, then the CaO. How long do you mix the CaO and how long do you leave it settle before you use it?

                        Tilly, the way I read it, I think Murfs referring to 55L batches of methoxide.

                        Thanks Wesley, the dessicant properties of CaO in alcohols is well documented as you have discovered. It does seem to take some time to adsorb the water and perhaps the exchange of info in this thread will be able to pin down how us biodiesel homebrewers can put it to good use.

                        Comment


                        • #57
                          Re: New Methods #2. The Imisides Method

                          Hi geewizztoo,
                          I think you are correct.
                          I have changed that part of my post.
                          Originally posted by geewizztoo View Post
                          Tilly, the way I read it, I think Murfs referring to 55L batches of methoxide.

                          Comment


                          • #58
                            Re: New Methods #2. The Imisides Method

                            Originally posted by tillyfromparadise View Post
                            Hi Murf,
                            Thank you for your reply.
                            Can you be more specific as to what tests you have performed.
                            Did you ever do a 3/27 test?

                            What formula do you use to make biodiesel?
                            In particular how much methanol and how much KOH and CaO do you use for each litre of oil reacted?
                            For instance, while Mark's instructions are a bit vague. as close as I can make out, Mark seems to recommend using 150ml methanol, 15g KOH and 30g CaO for each litre of WVO being reacted. That would work out to 15 litres of methanol per 100 litre of WVO being reacted.
                            I make 55lt batches of Methoxide in a 60lt home brew drum with a tap at the bottom

                            551t of Methanol

                            5.5kg of KOH
                            , I mix in 2.5kg one day and 3kg the next, it gets too hot if I put the 3kg in first

                            5kg of CaO quicklime is stirred in once it has cooled down, usually the next day (a good long stir)

                            then after a few days settling I decant off the Methoxide into 20lt plastic Jim Beam containers, I put 17lt into these containers as only 15lt drains out when level, with the remaining 2lt I use the very scientific method of that oil looks **** so I tilt the drum and pour an extra 1lt or so of Methoxide into the reactor. the CaO settles some more in the 20lt containers.

                            15lt of Methoxide to 100lt of 50deg Celsius WVO I never used to heat the oil at first but just got into the habit of heating in winter and just kept heating

                            mix through processor for one hour

                            drain off by-product

                            pump to 205lt open top drum
                            let settle for a few days, this drum has a stand pipe inside it so I can decant of the Bio and leave the residual by-product to be drained into a 20lt drum

                            gravity drain Bio to another 205lt open top drum
                            this drum also has a stand pipe inside it so I can decant of the Bio and leave the residual by-product

                            Air wash the Bio with a fish tank bubbler,
                            usually 3 to 5 days, this is the other very scientific method of a sniff soon tells you if it still has methanol in it

                            Pump up to 1300lt stand tank with gravity feed bowser,
                            I keep an eye on the settlement in this tank through the bottom drain I fitted a valve to and I get very little by-product
                            I also have a 205lt open top drum plumbed into the processor for settling oil, it has a stand pipe inside so I can decant off the settled oil and drain out any water and chips. I pump into this from my oil trailer tanks and also empty the dregs of the 20lt drums of oil into it

                            I use the processor pump to fill the processor from an open top drum at knee height, I pour 20lt drums of WVO into this keeping an eye out for the rubbish on the bottom that is then poured into the oil settlement tank

                            oh well back to the brew room to make some BIO and run the still for some moonshine

                            cheers Murf
                            3 years of BD100 using the Dr Mark Imisides method, currently making 10,000lt/year

                            1991 GQ Patrol 4.2 with DTS turbo

                            Comment


                            • #59
                              Re: New Methods #2. The Imisides Method

                              Did you ever do a 3/27 test?


                              yes in the early days and it passed no worries

                              I learnt what oil did what and just go by feel now

                              I don't spend a lot of time making BIO compared to some, I am human and very lazy and will take the path of least resistance

                              I have to use my Iphone timer to keep reminding me of the steps though, I learn't that the hard way

                              cheers Murf
                              3 years of BD100 using the Dr Mark Imisides method, currently making 10,000lt/year

                              1991 GQ Patrol 4.2 with DTS turbo

                              Comment


                              • #60
                                Re: New Methods #2. The Imisides Method

                                Hi Murf,
                                Originally posted by murf View Post
                                Did you ever do a 3/27 test?

                                yes in the early days and it passed no worries
                                That is interesting to hear.
                                Because you are evidently the only person to ever actually perform any testing with this procedure, Just to confirm that your fuel does pass the 3/27 test could you perform a 3/27 test on some of your biodiesel that you have in storage and report back your results.

                                3/27 test posted here


                                For years I used a similar fomula to the one you use use except I only used 6g NaOH mixed into 150ml methanol per litre of oil reacted and no CaO. That also made very nice biodiesel.

                                Comment

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