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Foolproof Room Temperature (FRT) Biodiesel

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  • Foolproof Room Temperature (FRT) Biodiesel

    Some years ago I introduced the "Imisides Method" - a foolproof means of manufacturing biodiesel. In retrospect the use of my name was probably a little self-indulgent, but was done simply because this is how things are done in the chemical literature (Grignard Reaction, Aldol Condensation etc). Thus it has now been renamed to make it descriptive of the process.

    In that time it has been through a few modifications and the volumes have now been optimised for the manufacture of 1080 L in an IBC

    I have now posted it on my website, complete with videos. You don't need to understand the chemistry of the process to make it work - this method is so simple that all you have to do is follow simple instructions (with help from the videos).

    So if you're wasting your time with titrations, or heating your process, you don't have to.

    For those in and around Perth, I'll be doing a public demonstration of it with my next batch, although that will be several months away.

    Please note that I won't be responding to any comments or questions on this forum, owing to the presence of a certain individual who ruins this site for everyone, and whose posts I stopped reading years ago.

    There is a facility on my website for asking questions or making comments, and any genuine questions or comments will be addressed there.

    Cheers
    Mark Imisides (aka Dr Chemical)
    Dr Mark
    Senior Member
    Last edited by Dr Mark; 30 January 2019, 08:12 PM.

  • #2
    Re: Foolproof Room Temperature (FRT) Biodiesel

    WOW! You have increased the KOH requirement from 15g KOH per litre of WVO to 20g KOH per litre of WVO!!

    I see you took my 2017 test results that I posted on this forum to heart that showed this "foolproof" procedure would not make biodiesel with oil titrating 18 KOH when using "only" 15g KOH per litre of WVO.
    I suspect that this new increased amount of 20g KOH per litre of WVO will still not make biodiesel with oil titrating 18 KOH.
    http://www.biofuelsforum.com/threads...s-method/page6

    You must be on a first name basis with your KOH supplier

    Comment


    • #3
      Re: Foolproof Room Temperature (FRT) Biodiesel

      Do the Brisbane and Perth football teams have supporters that are always 'falling out'!

      Comment


      • #4
        Re: Foolproof Room Temperature (FRT) Biodiesel

        Hi Smithy,

        Originally posted by smithy View Post
        Do the Brisbane and Perth football teams...
        When you say Football, do you mean Rugby Union, Rugby League, Australian Rules, Soccer, or Gridiron?

        Comment


        • #5
          Re: Foolproof Room Temperature (FRT) Biodiesel

          A Huge mistake in the instructions!!

          Hi Mark,
          I was really shocked to read in your instructions where you said;
          "The Dr Pepper method is constrained in the amount of catalyst it can add because of the danger of promoting saponification. So the mixture needs to be heated (to 55 deg C)."
          This statement is simply not correct. Everyone knows that there is no requirement to heat the oil before performing the reaction.
          It is common knowledge that when performing a single or multiple stage base reaction, the reaction works just fine at ambient temperature as long as everything remains liquid.
          I have told you this a number of times.
          Even your good friend WesleyB posted last year on this forum in the Imisides Method thread;
          "Well Tilly you're right. I reacted 380 milliliters Mazola new corn oil , titration number 0.13 with 100 milliliters methanol with 3.4 grams 85% potassium hydroxide dissolved in it, at a room temperature of twenty five degrees celcius,... did a Warnquest 10/90 test, there was no fallout. So, biodiesel transesterification reaction can be done without heating using the regular method"
          http://www.biofuelsforum.com/threads...ght=#post66002

          I think it would really help if you did some testing.
          If you need any further assistance please do not hesitate to ask.

          Comment


          • #6
            Re: Foolproof Room Temperature (FRT) Biodiesel

            Please note that my method has been updated:

            1. Extra videos have been added. In particular I have addressed the issue of waste disposal. One unexpected outcome of this method was a very low viscosity, low foaming glycerol phase that is easily disposed of down the sink.

            2. A calculation section has been added.

            Please note that only genuine questions or comments will be answered on this forum

            Comment


            • #7
              Re: Foolproof Room Temperature (FRT) Biodiesel

              Hi Mark,

              Originally posted by Mark View Post
              Please note that only genuine questions or comments will be answered on this forum
              Oh well, that is a change. You originally posted above; "Please note that I won't be responding to any comments or questions on this forum"

              Comment


              • #8
                Re: Foolproof Room Temperature (FRT) Biodiesel

                Lots of Soap Being Produced!

                Hi everyone,

                A few weeks ago Mark was involved in a discussion on the infopop forum concerning this room temperature “foolproof” procedure.
                During the discussion, RickDaTech told Mark that there was nothing new about performing the reaction at room temperature and Rick posted a link to a youtube video that showed a woman making biodiesel at room-temperature

                Mark then posted-
                Of more concern is the volume of glycerol. With my method, 17% methoxide by volume generates 22% glycerol by volume. In this video clip it's no more than about 10%. So at best it's a halfway reaction
                For some reason Mark erroneously equates lots of byproduct produced (Mark calls it glycerol) being an indication of a full reaction.

                It is not.
                Lots of byproduct (glycerol) is a sign of lots of soap being produced.

                I had posted the following to Mark earlier in that discussion;
                "For some reason you erroneously equate a large By-Product layer (that which you refer to as glycerol) as an indication of a "full" reaction. That is not the case.
                A large By-Product layer is an indication of a large amount of soap being produced.
                You say you produce about 22% By-Product
                Let me help you understand this.

                The By-Product layer (which you call glycerol) is usually composed of four main ingredients;
                Glycerol
                Methanol (with KOH)
                Soap
                Biodiesel

                It is easy to do a rough calculation of the quantities of each ingredient.

                Glycerol- There is about 79ml of glycerol in every litre of oil. That means in in a full reaction, the glycerol will be about 7.9% of the total volume of oil reacted which is about 6.6% of the total content volume of your reactor keeping in mind you added 17% methanol to the oil.

                Methanol
                - There is a rule of thumb that says that about 1/3 of the excess methanol is in the biodiesel phase and 2/3 of the excess methanol is in the By-product phase.
                The Stoichiometric amount of methanol for a complete reaction is considered to be about 12% of the volume of the oil. You used 17% (170ml per litre of oil) methanol in the reaction. That means there is an excess of 5% methanol that will be divided between the biodiesel and by- product phases.
                If 2/3 of this excess is in the byproduct, that is about 2.8% methanol of the total content volume in the reactor keeping in mind that you added 17% methanol to the oil.

                If you produced no soap, there would be virtually nothing else in the Byproduct Layer.
                In that case the By-Product Layer would be about 9.4% by volume of the total volume of the reactor..
                Testing I have done shows that this is pretty accurate.

                However, you say you have about 22% glycerol in the reactor
                So what is the additional 12.6% By-product you are producing?
                It is Soap and biodiesel
                The Rule of thumb here is that for every 1 litre of soap produced it will take about 2 litre of biodiesel with it into the By- product.
                So about 1/3 of the additional 12.6% by-product or about 4.2% of the total volume in the reactor is soap and about 8.4% is Biodiesel.

                So your byproduct layer ,expressed as a percentage of the total volume of the contents of the reactor contains about;


                Soap- 4.2%
                Glycerol- 6.6%
                Biodiesel- 8.4%
                Methanol- 2.8%


                As you can see, your by-product layer is actually only about 30% glycerol.

                I hope you have found this explanation helpful and has sorted out your confusion in this matter.
                Please do not hesitate to contact me if I can help clear up any other misunderstandings you have
                ."
                tillyfromparadise
                Senior Member
                Last edited by tillyfromparadise; 6 March 2019, 04:11 PM.

                Comment


                • #9
                  Re: Foolproof Room Temperature (FRT) Biodiesel

                  Tilly you wrote the glycerine produced in making biodiesel is about 7.9% of glycerol per litre of oil used. I calculated it myself but my calculation is 69 1/3 milliliters of glycerine produced per litre of liquid lard used to make biodiesel. Lard is a little different in its' average molecular weights of the free fatty acids present, but not that much. I got the theoretical stoichiometric amount of methanol was 115 milliliters of dry methanol per litre of oil used. Something is odd about getting a large glycerine layer. About 1/3 of excess methanol goes into the glycerine layer.

                  Comment


                  • #10
                    Re: Foolproof Room Temperature (FRT) Biodiesel

                    Note - I have now published an article describing the chemistry of the glycerol and soap phases. https://www.biofuelsforum.com/threads/11788-The-chemistry-of-the-glycerol-(and-soap)-phase?p=66419&posted=1#post66419

                    I've also updated the post on my website. The glycerol and soap phase is something that we normally don't pay much attention to. Soap formation is of course inevitable where you have FFAs and an alkaline environment. With this method it deposits out as a light brown gelatinous layer on top of the glycerol phase. What's intersting is that it only appears after the clarification process has run its course. That is, when all the excess MeOH has been evaporated off, the soap falls out of solution and settles on top of the glycerol.

                    The (obvious) advantage of this method of course is that it doesn't matter how much soap you form - as it's anhydrous there's no water to emuslify, so it just sits on top of the glycerol and gets tipped down the sink.

                    I'll post some pics later

                    Comment


                    • #11
                      Re: Foolproof Room Temperature (FRT) Biodiesel

                      Hi WesleyB,

                      Originally posted by WesleyB View Post
                      Tilly you wrote the glycerine produced in making biodiesel is about 7.9% of glycerol per litre of oil used. I calculated it myself but my calculation is 69 1/3 milliliters of glycerine produced per litre of liquid lard used to make biodiesel. Lard is a little different in its' average molecular weights of the free fatty acids present, but not that much.
                      I do not know why you have a different number. As I recall Neutral did specify there was about 79ml glycerine in a litre of WVO. If you do a google search, 79ml glycerine per litre of Veg oil is the number that is always quoted.


                      I got the theoretical stoichiometric amount of methanol was 115 milliliters of dry methanol per litre of oil used.
                      The stoicheometric amount of methanol depends on the oil in question. If you look at the chart below from the Journey to Forever site, it shows that it can vary from a low of 11.3% (113 ml) in the case of Rape/ Canola to a high of 16.3% (163ml) for coconut.
                      As most people do not know what oils are in their WVO, it is customary to consider the stoichiometrioc value for WVO around 12%- 12.5%



                      Oils and fats
                      Total
                      molecular weight
                      Density
                      Density
                      @ 50ºC
                      Volume
                      oil (ml)
                      Volume
                      methanol (ml)
                      Stoich. ratio
                      methanol : oil %
                      Tallow
                      858.54
                      0.895
                      0.88
                      981.18
                      121.52
                      12.4
                      Lard
                      863.73
                      0.92*
                      0.9*
                      959.7*
                      121.52
                      12.7
                      Butter
                      797.64
                      0.91
                      0.89
                      896.73
                      121.52
                      13.6
                      Coconut
                      674.51
                      0.926
                      0.91
                      744.57
                      121.52
                      16.3
                      Palm kernel
                      704
                      0.912
                      0.89
                      789.33
                      121.52
                      15.4
                      Palm
                      847.28
                      0.923
                      0.9
                      938.29
                      121.52
                      13
                      Safflower
                      879.1
                      0.927
                      0.91
                      966.44
                      121.52
                      12.6
                      Peanut
                      885.02
                      0.919
                      0.9
                      984.45
                      121.52
                      12.3
                      Cottonseed
                      867.38
                      0.918
                      0.9
                      963.76
                      121.52
                      12.6
                      Maize
                      872.81
                      0.923
                      0.9
                      966.57
                      121.52
                      12.6
                      Olive
                      870.65
                      0.923
                      0.9
                      964.17
                      121.52
                      12.6
                      Sunflower
                      877.22
                      0.925
                      0.91
                      969.3
                      121.52
                      12.5
                      Soy
                      882.82
                      0.925
                      0.91
                      975.5
                      121.52
                      12.5
                      Rapeseed/Canola
                      959.04
                      0.914
                      0.89
                      1072.75
                      121.52
                      11.3
                      Mustard
                      925.43
                      0.916
                      0.9
                      1032.85
                      121.52
                      11.8
                      Cod liver oil
                      908.81
                      0.929
                      0.91
                      1000.34
                      121.52
                      12.1
                      Linseed
                      872.4
                      0.934
                      0.91
                      954.48
                      121.52
                      12.7
                      Tung
                      873.68
                      0.944
                      0.92
                      945.54
                      121.52
                      12.9
                      * Approximate
                      Excess
                      tillyfromparadise
                      Senior Member
                      Last edited by tillyfromparadise; 6 March 2019, 10:17 PM.

                      Comment


                      • #12
                        Re: Foolproof Room Temperature (FRT) Biodiesel

                        Hi Wesley,

                        Originally posted by WesleyB View Post
                        About 1/3 of excess methanol goes into the glycerine layer.
                        That is not correct. Several people including me, have performed tests that shows that about 2/3 of the excess methanol is in the by-product (glycerine) and 1/3 is in the biodiesel.
                        If you leave it sit for a few days, even more methanol will accumulate into the by-product (glycerine) layer as the glycerine continues to settle out.
                        Methanol and glycerine are miscible in all proportions.
                        Methanol does not mix very well with biodiesel. That is why the 3-27 test works.
                        tillyfromparadise
                        Senior Member
                        Last edited by tillyfromparadise; 7 March 2019, 01:41 PM.

                        Comment


                        • #13
                          Re: Foolproof Room Temperature (FRT) Biodiesel

                          You're right Tilly about the 1/3 2/3 proportion in Biodiesel-glycerine excess methanol distribution. Sorry about that error. I try to be accurate. I have demethed crude biodiesel in a vaccum still before.

                          Comment


                          • #14
                            Re: Foolproof Room Temperature (FRT) Biodiesel

                            Hi Mark,

                            Originally posted by Mark View Post
                            Note -
                            The (obvious) advantage of this method of course is that it doesn't matter how much soap you form - as it's anhydrous there's no water to emuslify, so it just sits on top of the glycerol and gets tipped down the sink.
                            I'll post some pics later
                            There are several problems with this statement.
                            1. There will be water in the oil so this is not an anhydrous reaction
                            2. Of course it matters how much soap you form. The excess soap you produce directly reduces the biodiesel yield.
                            3.
                            Emulsions are not a concern when using KOH. I have never seen an emulsion form when using KOH in the reactor.
                            4. Every litre of soap produced combines with about 2 litres of biodiesel and takes it into the byproduct as well.

                            It would make much more sense to do a titration and determine the amount of KOH required for the reaction so as to avoid producing excess soap


                            tillyfromparadise
                            Senior Member
                            Last edited by tillyfromparadise; 12 March 2019, 03:49 PM.

                            Comment


                            • #15
                              Re: Foolproof Room Temperature (FRT) Biodiesel

                              I re did calculations for lard using an old organic chemistry book for free fatty acid lard composition. The internet gave density of lliquid lard as 917 grams per litre. So, The average molecular weight of free fatty acids in lard is 275 grams per mole. Average molecular weight of a lard triglyceride molecule is 863.3 grams per mole, which reacts with 129 milliliters of methanol per litre of lard stoichoimetrically to make biodiesel producing 77.6 milliliters of glycerine per litre of liquid lard. The 129 milliliters of methanol is per litre of liquid lard stoichiometric amount. Density of lard may vary some.

                              Comment

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