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  • The Imsides method

    On this forum a while back "the Imisides method" was explained. The concentration of methoxide ion was said to be increased by the use of calcium oxide in potassium or sodium hydroxide/methanol solution. But calcium soap also occurred as an additional product. Calcium soap (ring around the tub) is an added problem in purification of useable, premium quality fuel. Mark Imisides said the reaction proceeded faster at a lower temperature. I have some calcium oxide but chemicals are hard to get here in Texas. I had hoped to use it on a more valuable project.

  • #2
    Re: Reduced oil temperature in reactor ?

    Hi Wesley,

    Originally posted by WesleyB View Post
    Mark Imisides said the reaction proceeded faster at a lower temperature.
    Are you saying that you think the esterfication reaction goes faster the lower the temperature and all the chemists who have been advising that the warmer the temperature the faster the reaction have been making a mistake?
    Or are you talking about something entirely different that is not relevant to this discussion?

    Experiments I performed a number of years ago also showed that the warmer the reaction the quicker it went.

    Please provide us a link to the quote you are talking about.

    Comment


    • #3
      Re: Reduced oil temperature in reactor ?

      All i know is the extreme agitation and 60 degrees makes more (volumetricall fuel than original oil volume with obvious high conversion %, very sad problrm when your 1000 litres of oil makes more than 1000 litres of bio.
      Biodiesel Bandit

      Landcruiser '98 80 series B100.

      Comment


      • #4
        Re: Reduced oil temperature in reactor ?

        Matt. how did you determine it was "obvious high conversion%"
        I wouldn't complain if I were you.
        Life is a journey, with problems to solve, lessons to learn, but most of all, experiences to enjoy.

        Current Vehicles in stable:
        '06 Musso Sports 4X4 Manual Crew Cab tray back.
        '04 Rexton 4X4 Automatic SUV
        '2014 Toyota Prius (on ULP) - Wife's car

        Previous Vehicles:
        '90 Mazda Capella. (2000 - 2003) My first Fatmobile. Converted to fun on veggie oil with a 2 tank setup.
        '80 Mercedes 300D. 2 tank conversion [Sold]
        '84 Mercedes 300D. 1 tank, no conversion. Replaced engine with rebuilt OM617A turbodiesel engine. Finally had good power. Engine donor for W123 coupe. (body parted out and carcass sold for scrap.)
        '85 Mercedes Benz W123 300CD Turbodiesel
        '99 Mercedes W202 C250 Turbodiesel (my darling Wife's car)[sold]
        '98 Mercedes W202 C250 Turbodiesel (my car)[sold]
        '06 Musso Sports Crew Cab well body. [Head gasket blew!]
        '04 Rexton SUV 2.9L Turbodiesel same as Musso - Our Family car.
        '06 Musso sports Crew Cab Trayback - My hack (no air cond, no heater).

        Searching the Biofuels Forum using Google
        Adding images and/or documents to your posts

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        • #5
          Re: Reduced oil temperature in reactor ?

          Originally posted by WesleyB View Post
          On this forum a while back "the Imisides method" was explained. The concentration of methoxide ion was said to be increased by the use of calcium oxide in potassium or sodium hydroxide/methanol solution. But calcium soap also occurred as an additional product. Calcium soap (ring around the tub) is an added problem in purification of useable, premium quality fuel. Mark Imisides said the reaction proceeded faster at a lower temperature. I have some calcium oxide but chemicals are hard to get here in Texas. I had hoped to use it on a more valuable project.
          Hi Wesley< I don't remember mark imisides saying that a lower temperature was advantageous although I remember he did the process cold. Maybe this could be the subject of another Thread in order not to confuse the original question.

          Comment


          • #6
            Re: Reduced oil temperature in reactor ?

            Messaged moved
            Life is a journey, with problems to solve, lessons to learn, but most of all, experiences to enjoy.

            Current Vehicles in stable:
            '06 Musso Sports 4X4 Manual Crew Cab tray back.
            '04 Rexton 4X4 Automatic SUV
            '2014 Toyota Prius (on ULP) - Wife's car

            Previous Vehicles:
            '90 Mazda Capella. (2000 - 2003) My first Fatmobile. Converted to fun on veggie oil with a 2 tank setup.
            '80 Mercedes 300D. 2 tank conversion [Sold]
            '84 Mercedes 300D. 1 tank, no conversion. Replaced engine with rebuilt OM617A turbodiesel engine. Finally had good power. Engine donor for W123 coupe. (body parted out and carcass sold for scrap.)
            '85 Mercedes Benz W123 300CD Turbodiesel
            '99 Mercedes W202 C250 Turbodiesel (my darling Wife's car)[sold]
            '98 Mercedes W202 C250 Turbodiesel (my car)[sold]
            '06 Musso Sports Crew Cab well body. [Head gasket blew!]
            '04 Rexton SUV 2.9L Turbodiesel same as Musso - Our Family car.
            '06 Musso sports Crew Cab Trayback - My hack (no air cond, no heater).

            Searching the Biofuels Forum using Google
            Adding images and/or documents to your posts

            Comment


            • #7
              Re: Reduced oil temperature in reactor ?

              The concentration of methoxide is increased by calcium oxide absorbing water from the methanol, methoxide, potassium or sodium hydroxide solution. Water decomposes methoxide. It shifts the equilibrium to the right (products side of the sodium hydroxide + methanol yields methoxide + water) . By removing the water more methoxide forms at the same temperature resulting in a faster reaction.

              Comment


              • #8
                Re: Reduced oil temperature in reactor ?

                Tony, It's Imisides not Insides. Anyway just to add, when I tried this method coming up to 3 years ago using Potassium Methoxide dried by using quicklime (CaO) the volume of glycerol recovered after processing was greatly reduced. Glycerol has a variable soap content depending on oil quality, methanol quality and type of catalyst used, but is in the order of 35%. With the dry methoxide there was virtually no potassium soap, so the glycerol volume was about 2/3 of normal.

                Water washing was amazing, after the 1st wash the water was nearly clear. What lets this method down is the calcium soaps that are formed during the process. They are insoluble, so can't be removed by water washing. I tried the centrifuge and that also didn't work. I tried a magnesol treatment, also with a negative result. The only thing that worked was to filter the dried, slightly cloudy (due to calcium soaps) bio through oak chippings (3 times!) to get a zero soap result.

                My conclusion was that it is too much of a 'faf' on to process like this every time.

                Comment


                • #9
                  Re: Reduced oil temperature in reactor ?

                  Hi everyone,
                  There have been many glowing claims made for this method. Unfortunately, as far as I can tell, No one has ever actually performed careful controlled comparison testing to to find out what, if anything the benefits actually are.

                  Apparently this method removes water produced when mixing Methanol with KOH/ NaOH to produce the methoxide which should result in less soap being produced. Ideally this should give similar results to using Anhydrous Sodium Methylate (ASM)

                  During the base transesterification reaction, soap is produced in two ways.
                  I- Neutraliztion of FFA. This will happen regardless of the water content of the methoxide
                  2- Soponification of the oils because of water being present. This is dependent on water being present in the reaction. Reducing the water content of the methoxide should decrease the soap produced from soponification.

                  The theoretical maximum yield by volume using new oil with a titration of 0 is around 104%
                  I have seen claims of a volume yields greater than 100% using the standard single stage base method.
                  This suggests that provided the oil is dry there is actually very little soap produced through soponification as a result of the water produced when mixing methanol and KOH to produce the methoxide

                  It would be interesting to see some real meaningful test performed and their results
                  tillyfromparadise
                  Senior Member
                  Last edited by tillyfromparadise; 31 August 2017, 10:46 AM.

                  Comment


                  • #10
                    Re: Reduced oil temperature in reactor ?

                    Tilly; Making and curing soap can take days or months. Reaction rate is a factor in synthesizing biodiesel (30 minutes?). I made potassium soap (exothermic) via palm kernel (solid) flakes and potassium hydroxide pellets plus a little heat. I used a thermometer as a stir rod (carefully). Heating the mix a little the exothermic reaction wen't up to 170 degrees centigrade. I did not add water to the mix. I did that years ago. A very little bit of water causes the reaction to proceed but for a long time. So a little water in our transesterification biodiesel making reaction is relatively fast, not much soap has time to saponify. But the free fatty acids present can make soap with calcium (di) hydroxide to produce the ring around the tub, soap scum, calcium soap. So the Imisides method might be advantageous with dry vegetable oil low in free fatty acids, like new oil. I read removing calcium soap is difficult (3 times through wood chips). By increasing the methoxide concentration the reaction may proceed at lower temperatures (energy economics).

                    Comment


                    • #11
                      Re: Reduced oil temperature in reactor ?

                      Hi WesleyB

                      I make soap too!!

                      Indeed, the Imisides method MIGHT be advantageous in any number of ways.
                      The problem is that to date no one has ever presented any meaningful testing that demonstrates it has any advantage over the methods now in use.
                      I am assuming you have not performed any meaningful testing with the method and are just speculating what some of the benefits might be

                      Several thing come to mind when discussing water in the reaction.
                      NaOH typically contains less than 1% water while KOH typically contains 10%- 15% water, I have never seen anyone complain about having a reduced yield using KOH.

                      Also, many years ago there was a procedure that was popular called Cons Aqueous NaOH (Concentrated Aqueous NaOH).
                      This involved mixing the NaOH with an equal weight of water and then mixing that into the Methanol
                      That ended up putting 6ml- 10ml of water into the reaction for every litre of WVO being reacted.
                      That is a huge amount of water compared to the amount of water that might be produced when mixing NaOH/ KOH with methanol.

                      I used the Cons Aquous method until I changed over to using KOH.
                      Testing I did showed that using the Cons Aqueous method resulted in about a 1% reduction in yield by volume compared to not using the method.
                      The Chemist Neutral was not at all a supporter of the procedure and did some testing. He was quite amazed at how much soap was not produced using the Cons Aqueous method- "The loss is not as great as certain vocal critics asserted however, being less than 2% under typical conditions."

                      That tends to show that water in the reaction is probably not as big a problem as most people think it is.

                      I would love to see some well thought out testing performed using the above Imisides procedure
                      tillyfromparadise
                      Senior Member
                      Last edited by tillyfromparadise; 31 August 2017, 05:19 PM. Reason: Tidy things up

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                      • #12
                        Re: Reduced oil temperature in reactor ?

                        Hi Tilly, I'm assuming the advantage to the cons aqueous method is that the NaOH dissolves faster in water.

                        I have used reclaimed methanol that contained 1% water and found a yield loss of only 2 to 3 litres (compared to virgin) in a 200 litre batch.

                        Comment


                        • #13
                          Re: Reduced oil temperature in reactor ?

                          Tilly from Paradise, One of the smartest men I've met said, "the problem in science is not answering the (chemistry) question , but it's asking the right question". He was a theoretical chemist who did probability chemistry experiments on computer. So Tilly, how would you propose that the Imisides method be compared to plain transesterification reaction, one stage system, to show advantage?

                          Comment


                          • #14
                            Re: Reduced oil temperature in reactor ?

                            Hi Wesley,
                            One of the smartest men I have met said: "Never play another man's game"

                            Originally posted by WesleyB View Post
                            So Tilly, how would you propose that the Imisides method be compared to plain transesterification reaction, one stage system, to show advantage?
                            There seem to be several advantages claimed for the method. Which advantage do you wish to test for first?

                            PS One of the main claim seems to be that the Imisides method will make biodiesel at room temperature whereas the other procedures require heating.
                            As people have been producing biodiesel at room temperature for the last 15- 20 years using the single stage base method, I do not think we need to do much testing for that one
                            tillyfromparadise
                            Senior Member
                            Last edited by tillyfromparadise; 2 September 2017, 01:55 PM.

                            Comment


                            • #15
                              Re: Reduced oil temperature in reactor ?

                              I would want to test rapidity of reaction of new corn oil comparing potassium hydroxide transesterification with the Imisides method using potassium hydroxide at room temperature. A problem in producing synthetic fuel fuel (biodiesel) is how much energy is used to achieve a product versus how much energy is obtained when burning the fuel. If heating might be eliminated while still achieving a rapid reaction rate then at least for new corn oil with a titration of 0.6 (sodium hydroxide) that might be considered an advantage. New oil has low free fatty acid content and a minimal amount of calcium soap woul;d be produced. I only have one magnetic stirrer not two, to react them side by side.

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