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Thread: Glycerol composition.

  1. #51
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    Re: Glycerol composition.

    Tony, the only contaminate that would adversely affect the bio using methoxide dried with cement or CaO would be calcuim soap. This will only be present if some cement/CaO fines have found their way into the methoxide added to the oil.

    The reduction in glycerol volume is an indication that less soap has been produced. If glycerol is cracked with conc sulphuric the top FFA layer formed is an indication of the original soap content of the glycerol, which is on average in the order of 35% by volume. Do this test with glycerol from dry oil and methoxide ex the imisides drying method and the FFA layer is virtually non existant.

  2. #52
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    Re: Glycerol composition.

    Hi smithy,

    Quote Originally Posted by smithy View Post
    Tilly, the CaO amount is contained under the heading 'clinker' it will be similar to the 63% I posted above, otherwise any buildings made from cement with the CaO content you suggested would fall down!
    You seem confused.
    We are concerned with the amount of "free CaO" available in our bag of finest Grey cement, NOT the amount of CaO that is used to produce the cement.

    Burning in a kiln – formation of cement clinker

    Solid state reaction zone (900˚ - 1300˚)
    CaO and reactive silica combine to form small crystals of belite, one of the four main cement minerals.


    Clinkering zone (1300˚C – 1550˚C)
    Inside the liquid phase, Alite forms by reaction between Belite crystals and CaO.
    Crystals of solid Alite
    grow within the liquid, while crystals of Belite formed earlier decrease in number but grow in size.
    The clinkering process is complete when all of silica is in the Alite
    and Belite
    crystals and the amount of free lime (CaO) is reduced to a minimal level (<1%).

    Chemical composition of clinker
    The cement clinker formed has the following typical composition:
    Compound Formula Shorthand form % by weight1
    Tricalcium aluminate Ca3Al2O6 C3A 10
    Tetracalcium aluminoferrite Ca4Al2Fe2O10 C4AF 8
    Belite or dicalcium silicate Ca2SiO5 C2S 20
    Alite or tricalcium silicate Ca3SiO4 C3S 55
    Sodium oxide Na2O N ) )Up to 2
    Potassium oxide K2O K
    Gypsum CaSO4.2H2O CSH2 5


    Think of making glass
    While you start out with mostly sand in the furnace, there is very little sand left when you finish
    Last edited by tillyfromparadise; 24th December 2017 at 09:21 PM.

  3. #53
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    Re: Glycerol composition.

    Hi Tony,

    Quote Originally Posted by Tony From West Oz View Post
    Less byproduct may indicate greater yield, but what about quality?
    Byproduct = Glycerol, soaps, residual methanol, unused caustic, water (from the reaction) and other contaminants in the oil.
    What has been reduced in your "glycerol"? to reduce the volume you measured from this batch?
    The problem is the continual pretending that the glycerol prewash is not a stage of reaction.
    When the first stage of reaction performed is a glycerol pre wash where neither the amount of chemicals used in this first stage is measured or known and the byproduct/ glycerol (soap and glyerine) produced during this first stage are also unknown, the amount of byproduct/ glycerol produced in subsequent stages has no meaning.

    Also, because there is biodiesel bound with the glycerol used to perform this first stage and an unknown amount of this biodiesel is released into the reactor, yield is not measurable.
    Last edited by tillyfromparadise; 24th December 2017 at 03:44 PM.

  4. #54
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    Re: Glycerol composition.

    Hi smithy,
    Quote Originally Posted by smithy View Post
    The reduction in glycerol volume is an indication that less soap has been produced. If glycerol is cracked with conc sulphuric the top FFA layer formed is an indication of the original soap content of the glycerol, which is on average in the order of 35% by volume.
    The problem here is that you pretend the glycerol pre-wash is not a stage of reaction and you do not include the soap or the glyceine produced during this first stage reaction when you do your testing.

    Have another look at the test results DavidS reported to refresh your memory of the difference between dried and non-dried methoxide

    HINT: No matter what magical procedure you use, FFA's will NOT be converted into biodiesel in a Base only reaction

    Smithy, you have still not explained how you achieve a full conversion in a single stage reaction on WVO using just 12% methanol.
    I am sure all the people who you claim are reluctant to join in this discussion for fear of being humiliated are desperate to know how you achieve this seemingly impossible feat.
    Please tell us how you do this.


    "I appreciate your effort here but you consistently get results that no one else can achieve due to unknown circumstances, because of this your results dont hold much weight."
    Last edited by tillyfromparadise; 24th December 2017 at 03:45 PM.

  5. #55
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    Re: Glycerol composition.

    I'll handle some of the info posted by Tilly in due course . Too busy getting ready for Christmas Day at the moment, but for now:

    Clinker Composition

    In cement chemistry, chemical analyses are normally given in oxide form - a typical example of an analysis follows:
    Typical clinker analysis (oxide weight%).
    SiO2 Al2O3 Fe2O3 CaO MgO K2O Na2O SO3 LOI IR Total
    21.5 5.2 2.8 66.6 1.0 0.6 0.2 1.0 1.5 0.5 98.9
    Free lime = 1.0% CaO
    Balance is typically due to small amounts of oxides of titanium, manganese, phosphorus and chromium.
    From the chemical analysis, the quantity of each of the four main minerals can be calculated using the 'Bogue' calculation (click on the link below for more information.)

  6. #56
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    Re: Glycerol composition.

    Hi smithy,

    Smithy posted:
    Free lime = 1.0% CaO
    1% free CaO sounds about right- perhaps a tad higher than desired but close enough.
    As I mentioned in an earlier post in this thread, the MSDS for Grey cement lists the CaO content as 0- 1%
    "The free CaO (often called the “free lime”) is the amount of calcium oxide present as CaO, that is, not bound into the cement minerals"

    It is good to see that you agreeing with me

    The great majority of CaO used to produce Cement Clinker is "used up" during the sintering process to produce Alite and Belite so there is virtually no CaO available to remove water during the drying of the methoxide.

    Merry Christmas
    Last edited by tillyfromparadise; 24th December 2017 at 11:46 PM.

  7. #57
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    Re: Glycerol composition.

    Hi Tilly and Merry Christmas to you.


    Even at only 1% free CaO, there was a difference in the tests I ran previously. Perhaps I should do it again using CaO instead of the cement as the "drying agent". I have some CaO in a sealed tub.


    Best wishes


    David

  8. #58
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    Re: Glycerol composition.

    Hi DavidS,

    Quote Originally Posted by DavidS View Post
    Even at only 1% free CaO, there was a difference in the tests I ran previously. Perhaps I should do it again using CaO instead of the cement as the "drying agent". I have some CaO in a sealed tub.
    Yes, there was a difference.
    Because there is virtually no free CaO in cement to do the drying, it is very likely that one of the minerals produced during the sintering procedure is actually removing the water.
    As I recall, I also pointed out the lack of free CaO in cement to the author of this drying procedure and his reply was that it did not really matter what it was in the cement that was removing the water as long as it did not also remove methanol.

    My guess is that the difference in the batches was mostly because the drying procedure removed the 10% water in the KOH and not so much the removal of the small amount of water produced making Methoxide.

    Water is only produced when you mix KOH or NaOH with methanol if Methoxide is actually produced
    The chemist Neutral said that he thought there is actually very little methoxide produced when you mix KOH or NaOH with methanol and what we actually have is mostly just KOH or NaOH dissolved in methanol with a small amount of methoxide produced. Dissolving KOH or NaOH in methanol does not produce water, it is the production of methoxide that produces water.

    It would be interesting to see what happens if NaOH, which typically contains virtually no water, were used in the comparison test instead of KOH

    Merry Christmas to you too!
    Last edited by tillyfromparadise; 25th December 2017 at 06:46 AM.

  9. #59
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    Re: Glycerol composition.

    Hi everyone,
    Before Christmas we were discussing caustic stripping and in particular, the instructions in Paul Martin's book "Grown Fuel Biodiesel in practice"
    At the time I did question whether the instructions posted were accurate because they seemed to require a substantial excess of KOH.
    So I sent Paul an email querying the instructions as presented to this forum and I went to the local Paradise library and arranged for the book in question to be sent from the Gold Coast on an inter library loan.
    So far, Paul has not responded to my email.
    The book arrived at our library yesterday. The following are the instructions posted on page 18 of the 2008 edition of the book

    Removing Free Fatty Acids (FFAs)

    Only try this when you have been making biodiesel successfully for many months. It is a process that needs to be adjusted to suit, it can help or create a mess if you are not careful
    FFAs can be neutralised first to improve yield. Try stripping them from feedstock by adding a mixture of potassium hydroxide (KOH) and water to the feed stock.
    1. Determine the amount of KOH to add by titrating (See page 20) This time however, use the following formula:
    KOH in grams= (3.5+Y) x feedstock volume in litres.
    2. Measure out 40ml of water for every litre of feedstock and bring to the boil
    3. Add the required amount of KOH to the water.
    4. Ensure the feedstock is heated to 40C, then mix in the water/KOH mixture.
    5. Allow soaps to settle overnight.
    6 Titrate again to observe a reduction in catalyst needed for the batch.


    I still have serious doubts about these instructions- especially as it seems to require the addition of the KOH to BOILING water!

    Last edited by tillyfromparadise; 10th January 2018 at 01:20 PM.

  10. #60
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    Re: Glycerol composition.

    That is interesting, I have the 2006 edition 3 and everything is the same except you add NaOH to the boiling water. I still have not received my new book, and he hasn't responded to my email either. In practice I use hot water out of the safety valve on the hot water cylinder so around 60C and it works just fine.
    I'm a bit hesitant to do another batch of cement diesel as I still don't know what that white stuff is that drops out with the 10/90 test.It did work well though and I did get a little more bio and a little less glysterne

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