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Thread: The Imsides method

  1. #141
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    Re: Reduced oil temperature in reactor ?

    Quote 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

  2. #142
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    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.

  3. #143
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    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.
    Regards,

    Cade.

    2002 Landcruiser HZJ105r (1HZ motor) 250,000 on bio (sold)
    2006 Mazda B2500 (WLT motor) 80,000 on bio (sold)
    2006 Ford Courier(WLT Motor), just purchased


  4. #144
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    Re: Reduced oil temperature in reactor ?

    Hi Cade,

    Quote 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

  5. #145
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    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
    Last edited by tillyfromparadise; 8th June 2018 at 05:21 PM.

  6. #146
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    Re: Reduced oil temperature in reactor ?

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

  7. #147
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    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.

  8. #148
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    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.

  9. #149
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    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.
    Last edited by tillyfromparadise; 19th June 2018 at 04:36 PM.

  10. #150
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    Re: Reduced oil temperature in reactor ?

    Initially I put 13 grams calcium oxide + 11 grams 85% potassium hydroxide and 330 milliliters technical grade methanol into a 500 milliliter flask fitted for magnetic stirring. I made more methoxide solution than I would need. I stirred a bit from time to time to try to dissolve all the potassium hydroxide. Previously I tested new Mazola (name brand) corn oil for free fatty acids, I got 0.6 grams sodium hydroxide per litre to neutralize them. So I used magnesol XL to treat 700 milliliters of new corn oil thinking that might remove the free fatty acids (a small quantity). Eighteen hours (about) after I mixed the methoxide solution, I decanted off 100 milliliters of the upper clear liquid leaving the white solid in the mixing flask. I avoided putting the white solids into the vegetable oil. Mixing the 100 ml methoxide and 380 ml corn oil was done at room temperature of 22 degrees centigrade in a 1 litre glass storge bottle with a teflon cap. I shook it a few seconds , it separated that time. About one minute later I shook it a few seconds again, there was a noticeable color change and it did not separate quickly. Within about 15 minutes at room temperature a brownish glycerine layer was forming. The larger upper layer was transluscent. About 8 hours later I removed the glycerine layer in a separatory funnel ,then I washed (extracted) 5 times with distilled water. I got about 360 milliliters of wet biodiesel , added 40 grams anhydrous sodium sulfate (a drying agent). At 5PM the next day decanted off somewhat dried transluscent biodiesel. Added 25 grams magnesium silicate to remove more polar chemicals from the biodiesel with 60 degree centigrade heat on a hot plate with stirring. The biodiesel became transparent. Did a 10/90 Warnquest miscibility test there was no fall out. did a soap test but there seems to have been no soap in it at all, the biodiesel did not turn the bromophenol blue indicator blue for the test.
    Last edited by WesleyB; 20th June 2018 at 12:37 PM.

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