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  • Re: Reduced oil temperature in reactor ?

    Hello Tilly


    Leaving this test aside, if your assertion is correct that drying the methoxide has little benefit to the reaction, how come commercial producers and a fair few home producers in the UK swear by using ASM (anhydrous sodium methoxide) rather than mixing their own methoxide using the much cheaper sodium hydroxide in crystal form?


    Regards,


    David

    Comment


    • Re: Reduced oil temperature in reactor ?

      Originally posted by Tilly

      PS:

      By the way, I think that DavidS designed a very good test to compare the imsides procedure which dries the methoxide with the a procedure that does not dry the methoxide. I believe his results are valid.
      I think both you and Wesley need to have a good close look at how DavidS designed his COMPARISON TEST for your future reference
      -----------
      Originally posted by David S


      Hi Tilly,

      i will reply regarding my methoxide mixing a bit later today. I'm just going out to collect some oil.

      in fairness, I think if you look at my post #115 on this thread you will see that Dave (Smithy) actually suggested to me the way to run this test on new oil, using the same batch of methoxide and just changing one thing (addition of cement to the second test methoxide). Please give him credit for the scientific method that was applied to this testing.

      David

      ----------------------------------------------------
      Hmm, seems you have shot yourself in the foot with this one, Tilly!

      Comment


      • Re: Reduced oil temperature in reactor ?

        Hi David,



        Originally posted by DavidS View Post
        Hi Tilly,
        in fairness, I think if you look at my post #115 on this thread you will see that Dave (Smithy) actually suggested to me the way to run this test on new oil, using the same batch of methoxide and just changing one thing (addition of cement to the second test methoxide). Please give him credit for the scientific method that was applied to this testing.
        David
        It is heartening to see that smithy actually understands the concept of scientific testing.

        I give credit to smithy for advising you to use a scientific method in your test.
        I hope that in the future smithy will apply this same rigorous scientific method to his own testing and stops posting all the false and misleading information he currently posts.


        A few observations about your testing.

        I think your test results are valid.

        While I have never been terribly concerned with producing very high conversion biodiesel in a single stage using an absolute minimum of methanol possible, I have read of people achieving a pass on the 3/27 test using 16% methanol in a single stage reaction.

        It is interesting to see that your reaction went so far using 15% methanol.
        A few reasons that probably contributed to this-
        1. Your choice of oil was important.
          The stoichieometric amount of methanol for Rape/ Canola is not 12.5% as with most vegetable oil, it is actually only 11.3%. This means that you have a greater excess of methanol available when reacting rape/ canola than if you reacted almost any other oil using the same amount of methanol so the reaction will go farther.
        2. The oil was new.
        3. Testing I performed years ago showed that if you increased the NaOH in the reaction you could reduce the methanol and still achieve the same reaction results.
          I assume the same thing will happen when using a huge excess of KOH



        Leaving this test aside, if your assertion is correct that drying the methoxide has little benefit to the reaction, how come commercial producers and a fair few home producers in the UK swear by using ASM (anhydrous sodium methoxide) rather than mixing their own methoxide using the much cheaper sodium hydroxide in crystal form?
        I was basing my statement on your test results.
        As I recall the theoretical maximum yield by volume is about 104%
        Your non-dried batch achieved 103.9% yield.
        There does not seem to be a lot of room for more gain.

        You will need to ask the people who use ASM why they use ASM. I am sure they have a reason

        CONCLUSSION
        This procedure does seem to offer a benefit if you are attempting to produce high conversion biodiesel.
        It would be interesting to see what the results are when reacting WVO.
        I think it is amusing that the author of this procedure does not consider that conversion is important

        Well done on the test DavidS
        tillyfromparadise
        Senior Member
        Last edited by tillyfromparadise; 27 November 2017, 10:32 AM.

        Comment


        • Re: Reduced oil temperature in reactor ?

          Originally posted by DavidS View Post
          I calculated the mix for the methoxide as follows:


          Dr.Mark's bulk formula calls for 870lites of wvo to be reacted with a methoxide comprising 130ml of methanol plus 13kgs of KOH.
          Um that has gotta be a typo ..... correct?

          Otherwise 130ml of methanol would hardly even wet 13kg of KOH, let alone dissolve it.

          Comment


          • Re: Reduced oil temperature in reactor ?

            My bad. Apologies. I've now edited the post to read 130 litres.

            David

            Comment


            • Re: Reduced oil temperature in reactor ?

              Originally posted by DavidS View Post
              My bad. Apologies. I've now edited the post to read 130 litres.

              David

              No worries David. I thought you meant litres, and not ml.

              Had to get in before Tilly saw that LOL.

              Comment


              • Re: Reduced oil temperature in reactor ?

                Originally posted by tillyfromparadise View Post
                You will need to ask the people who use ASM why they use ASM. I am sure they have a reason
                Hi Tilly,


                Firstly, you were correct in that the new oil I tested was rape-seed oil.


                I use both sodium and potassium for processing. I buy the sodium from our local hardware chain (called Wilkos), who sell it packaged as drain cleaner, and it costs around £2 for 500g. I've always had difficulty getting the stuff to fully dissolve in methanol, and however long I leave it and however much I agitate it there always seems to be an amount that remains undisolved. I asked Dave about this the last time I saw him, and he suggested that it could be that the sodium packaged and sold as drain cleaner in the hardware stores contains some insoluble impurities, which seems a reasonable explanation. In any case, it still works when I add the resultant methoxide to my processor.


                Turning to the question I asked you - (why do people use ASM) - I think that its easy disolvability is one of the main reasons. If you look at this link (http://www.biopowered.co.uk/wiki/Anh...dium_methylate) which is from the Biopowered Wiki page, the advantaged and disadvantages are listed as follows:




                The pros and cons of using anhydrous sodium methylate
                Pros
                Mixing it with methanol is as easy as making orange squash
                Being a liquid, there is no corrosive dust to worry about
                Being around 70% methanol, using methylate requires less methanol in the batch
                Cons
                Methylate is considerably more expensive than solid catalysts although this can be offset against methanol savings
                Availability is still an issue although this is improving


                The "pros" do not list increased yield / conversion or decreased soap production as advantages, although I do seem to think that I have read users report that this is the case.


                I have used ASM before, and I have recently bought some more because I did like it, if only for the ease of mixing. It certainly is more expensive, but it is convenient and a time saver. I'd reserve judgement on whether it results in a "better" process than methoxide made using the standard sodium crystals.


                Best wishes,


                David

                Comment


                • Re: Reduced oil temperature in reactor ?

                  Hi Guys
                  I've made a mod to this method after some quantitative measurements. I've decided tu increase the methoxide ratio from 100:15 to 100:20. This accounts for the amount of MeOH that is consumed by the drying process - something I'd never measured before. In fact the leftover meOH was probably below the stoichiometric amount. With the old ratio of 100:15 it's likely that I wasn't getting complete conversion and there was probably a significant amount of unreacted WVO in there.

                  With the new quantities I'm getting more glycerol, and it's taking longer to remove the MeOH, so I'm sure it's now fully converted.

                  Comment


                  • Re: Reduced oil temperature in reactor ?

                    Bang on bro. I have been using 20% for 10 years with the knowledge that:

                    A. it works.
                    B. there was excess meth available in the reaction to account for water in meth and used oil.

                    I would bet my butt (and there is a lot of butt to bet) that a 200 litre drum of meth contains a fair whack of water. If you use WVO that has been used to fry chicken, man there is a lot of water in that oil.

                    My experience supports your calculations.

                    Comment


                    • Re: Reduced oil temperature in reactor ?

                      Hi Cade,

                      Originally posted by Captaincademan View Post

                      I would bet my butt (and there is a lot of butt to bet) that a 200 litre drum of meth contains a fair whack of water.
                      I use Rechochem methanol. Their MSDS says the purity is > 99%.
                      That would give less than 2 litres of water in a full 200 litre drum of methanol.

                      If you leave the drum of methanol outside in the rain with a lose top that could lead to a problem

                      Comment


                      • Re: Reduced oil temperature in reactor ?

                        Hi Mark,

                        I've made a mod to this method after some quantitative measurements.
                        I've decided tu increase the methoxide ratio from 100:15 to 100:20.
                        This accounts for the amount of MeOH that is consumed by the drying process - something I'd never measured before.
                        It is good to see you are finally doing some actual testing!
                        WELL DONE!!!

                        What you are saying does not add up.
                        You say you have increased the methanol from 150ml per litre of WVO to 200ml methanol per litre of WVO just to make up for the methanol that is bound up in the Cement powder during the drying phase and is no longer available to take part in the reaction.

                        In my experience when I was testing this method, while there seemed to be a small amount of methanol bound up with the Cement powder, it was nothing even remotely approaching 1/3 of the total volume of methanol being dried

                        If you were only concerned with replacing the methanol bound up in the cement powder, I think an extra 10ml methanol per litre of WVO would more than make up for the small amount of methanol removed with the cement powder.

                        Please describe the tests you performed that showed that for every 150ml of methanol you dried, 50ml of the methanol was bound up with the cement powder and removed from the reaction.




                        In fact the leftover meOH was probably below the stoichiometric amount.
                        If you were actually removing 50ml of methanol from every 150ml of methanol you were drying then you would have only been left with 100ml of methanol for each litre of WVO.
                        The stoichiometric ratio of methanol ranges from around 11.8% to 16.3% for most veg oils. The veg oil we are likely to use is around 12.5% (125ml methanol/ litre WVO)




                        With the old ratio of 100:15 it's likely that I wasn't getting complete conversion and there was probably a significant amount of unreacted WVO in there.
                        With the new quantities I'm getting more glycerol, and it's taking longer to remove the MeOH, so I'm sure it's now fully converted.
                        Wow, you seem to have done a 180 degree about face concerning conversion and now seem to think that conversion is important.
                        From the time you first posted this procedure in 2011 you have continually claimed that conversion was unimportant:
                        November 2011 you posted:
                        "And remember, the bio process is about one thing only - reducing viscosity. If you have incomplete conversion it doesn't matter, as we know that diesel motors run fine on WVO anyway as long as it's thin enough."

                        December 2011 you posted:
                        “One other thing - there is a lot of talk on this site about the 3/27 test, as though it's important.
                        It's not.
                        Making biodiesel is all about one thing - reducing viscocity. It doesn't matter if you have unconverted triglycerides in your fuel.”

                        March 2017 in the Warnqvest test and reprocessing thread you posted:
                        “This test is completely unnecessary. You are making fuel, not a pure laboratory product. Using biodiesel, instead of WVO, is all about viscosity. The efficiency of conversion is therefore immaterial.”

                        I am curious why you now seem so keen to achieve a "full Conversion"



                        With the new quantities I'm getting more glycerol, and it's taking longer to remove the MeOH, so I'm sure it's now fully converted.
                        I assume when you say “Glycerol” you actually mean “by-product”
                        The amount of glycerol/ by-product produced is not an indication of how “Full” the conversion is.

                        The amount of by-product is variable depending on, but not limited to:
                        Type of oil being reacted
                        Percent of conversion
                        The Titration of the oil
                        The amount of methanol used in the reaction
                        The amount of water in the reaction
                        The amount of caustic used in the reaction.
                        The radio station you are listening to.

                        If you need any further assistance with this please do not hesitate to ask
                        tillyfromparadise
                        Senior Member
                        Last edited by tillyfromparadise; 8 June 2018, 05:21 PM.

                        Comment


                        • Re: Reduced oil temperature in reactor ?

                          Dr. Mark; Have you done a 10/90 test? What were the results?

                          Comment


                          • Re: Reduced oil temperature in reactor ?

                            September 23 of last year I used Calcium Oxide to dry methanol, then used that methanol + potassium hydroxide catalyst , and magnesium silicate treated new corn oil to make biodiesel at room temperatature of about 21 degrees centigrade. I haven't found my lab notes on that one but when I do a 10/90 test now there is no fall out, in the Warnquest test.

                            Comment


                            • Re: Reduced oil temperature in reactor ?

                              I treated 700 milliliters of new corn oil with Magnesol XL at about 60 degrees centigrade. Magnesol may remove free fatty acids from new vegetable oil. I dried methanol with calcium oxide with enough potassium hydroxide in it to figure 7.4 grams per litre of vegetable oil. Put 380 millilitres Magnesol treated corn oil into a 1 litre storage bottle added 100 milliliters dried KOH methoxide soultion to the oil. Shhok the glass storage bottle. After shaking it a second time a noticeable color change occurred. Room temperature was 22 degrees centigrade. After about 15 minutes what might have been a glycerine layer began to form. 2 1/2 hours after mixing the chemicals a browninsh glycerine layer formed. 10 hours after initially mixing the chemicals at room temperature I extracted (washed) 5 times with distilled water. Added 40 grams of anhydrous sodium sulfate powder (a drying agent) to the biodiesel. The next day decanted the somewhat dried biodiesel into a clean beaker. Added 25 grams magnesium silicate to the biodiesel with stirring. Within 10 minutes I got a transparent yellow biodiesel product. I did a 10/90 Warnquest miscibility test, there was no fallout of unreacted corn oil. Dr Imisides suggested drying the methoxide solution with calcium oxide it worked on my small scale test. Using Magnesol to remove free fatty acids from the starting material might have helped too, it worked.

                              Comment


                              • Re: Reduced oil temperature in reactor ?

                                Hi Wesley,



                                I treated 700 milliliters of new corn oil with Magnesol XL at about 60 degrees centigrade. Magnesol may remove free fatty acids from new vegetable oil...
                                Every time I have titrated new veg oil it titrates around 0. Did you titrate this new corn oil before treating it with Magnesol?

                                It is easy to check whether Magnesol removes FFA's from the oil. Titrate the oil before performing the magnesol treatment and then titrate the oil after the magnesol treatment.
                                If there is a difference in the before and after titration number you will know if the magnesol removes FFA's from the oil







                                I dried methanol with calcium oxide with enough potassium hydroxide in it to figure 7.4 grams per litre of vegetable oil. Put 380 millilitres Magnesol treated corn oil into a 1 litre storage bottle added 100 milliliters dried KOH methoxide soultion to the oil.
                                This part is confusing.

                                You say you reacted 380 ml corn oil (38% of a litre of corn oil) with 100ml methoxide.
                                That means there would be about 38% of the 7.4g KOH you needed for a full litre of Corn oil in the 100ml of methoxide actually used
                                This is about 2.8g KOH mixed into the 100ml methanol.


                                Can you please be specific as to the total quantity of methanol you mixed with the total quantity of KOH from which you obtained the 100ml methoxide that you performed the reaction with.
                                tillyfromparadise
                                Senior Member
                                Last edited by tillyfromparadise; 19 June 2018, 04:36 PM.

                                Comment

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