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Thread: The Imsides method

  1. #71
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    Re: The Imsides method

    An answer to my own question-

    "Specific compounds dried with calcium hydride and analyzed for residual water content include benzene,2 dioxane,2 acetonitrile,2,4 methanol,5 ethanol,5 2-butanol5 and t-butyl alcohol...

    Methanol and ethanol are dried to ~100 ppm residual water content,5 in conflict with an early recommendation against using this drying agent.6 Apparently, calcium hydride reacts with water considerably faster than with alcohols, making it an excellent drying agent for these compounds."

    http://reag.paperplane.io/00000531.htm

    So apparently calcium hydride does dry methanol


  2. #72
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    Re: The Imsides method

    We learn something every day. Isn't that right Tilly?
    Life is a journey, with problems to solve, lessons to learn, but most of all, experiences to enjoy.

    Current Vehicles in stable:
    '85 Mercedes Benz W123 300CD Turbodiesel single tank using 95% used cooking oil and 5% to 10% misfuel (where someone had filled diesel vehicle with petrol).
    '06 Musso Sports Crew Cab. Running on used cooking oil with 5% to 10% misfuel.
    Toyota Camry Hybrid - (Wife's Car)

    Previous Vehicles:
    '90 Mazda Capella. (2000 - 2003) My first Fatmobile. Converted to fun on veggie oil with a 2 tank setup. Died when supercharger stuck at max boost for weeks. Stretched head bolts.
    '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. Donor for current Fatmobile coupe. (body parted out and carcass sold for scrap.)
    '99 Mercedes W202 C250 Turbodiesel (my darling Wife's car)[sold]
    '98 Mercedes W202 C250 Turbodiesel (my car)[sold]



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


  3. #73
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    Re: The Imsides method

    In organic reactions often a general reaction applied to a specific reaction applies to many other similar reactions. Calcium oxide adsorbing water from ethanol probably means it will absorb water from other alcohols with carbon carbon single bonds , like ethanol, propanol butanol isopropanol et cetera. So it probably adsorbs water from methanol (a similar reaction) producing calcium di hydroxide. Calcium oxide is a base. A base is a proton accepter. An acid is a proton donor. Calcium oxide, with one calcium atom and one oxygen atom accepts a hydrogen atom from water (the proton) making briefly calcium hydroxide with a positive charge, then the residual hydroxide from the acidic water losing a hydrogen atom quickly bonds with calcium hydroxide + to make calcium with two hydroxides bonded to opposite sides of the calcium atom. I did not copy that out of a book.

  4. #74
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    Re: The Imsides method

    RE-PROCESSED TITRATION 10 KOH BATCH- ACHIEVED SEPARATION

    Hi everyone,
    I did a reprocess of the 10 KOH titration batch using 6 KOH mixed into 50ml methanol and achieved separation.


    CONCLUSION

    We finally made biodiesel.
    So far I do not see any benefit in this procedure over the standard single stage method

  5. #75
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    Re: The Imsides method

    Tilly ; Calcium hydride is not the same thing as calcium oxide or calcium hydroxide or calcium dihydroxide. Calcium hydride is one calcium atom bonded to two hydrogen atoms. The formula would be Calcium (1) Hydrogen (2) or CaH2. I expect it is made by heating pure calcium metal with hydrogen gas molecules under high pressure. A more common example of a hydride is Lithium Aluminum Hydride. It is used to hydrogenate (add hydrogen to) some organic molecules . I think the formula is LiAlH4, Lithium (1 atom) Aluminum (1 atom) Hydrogen (4 atoms) That's one atom of lithium , one atom aluminum and four atoms of hydrogen all bonded together in one molecule.
    Last edited by WesleyB; 7th November 2017 at 12:30 AM.

  6. #76
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    Re: The Imsides method

    Quote Originally Posted by tillyfromparadse[SIZE=3
    So apparently calcium hydride does dry methanol[/SIZE]
    Indeed it does Tilly, which is why the Sandy Brae works to quantify the amount of water in methanol.

    Calcium Oxide also reduces the water in methoxide, I did a few water tests before and after adding CaO to prove this some years ago.
    Last edited by smithy; 7th November 2017 at 05:47 AM. Reason: spelling mistakes (naughty boy!)

  7. #77
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    Re: The Imsides method

    Hi smithy,

    Quote Originally Posted by smithy View Post
    Indeed it does Tilly, which is why the Sandy Brae works to quantify the amount of water in methanol.
    Calcium Oxide also reduces the water in methoxide, I did a few water tests before and after adding CaO to prove this some years ago.

    The Sandy Brae test kit does not claim to be able to detect water in methanol and Calcium oxide is not part of the Sandy Brae test kit.
    The Sandy Brae test kit detects water in oil using calcium hydride


    Last edited by tillyfromparadise; 7th November 2017 at 04:33 PM.

  8. #78
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    Re: The Imsides method

    That isn't what i said, Tilly. I was agreeing with you that calcium hydride can dry methanol, the very reason it works in the Sandy Brae, producing Hydrogen. I didn't mention anything about Calciom Oxide in the S/B.

    Just because Graydon doesn't mention anything in the S/B instructions about methanol doesn't mean it won't work. It does work accurately to evaluate the water content of methanol. I have had conversations with Graydon who agrees with me.

    It is the Carbide Manometer (updated by your mate IMB) that is incapable of measuring water in methanol.

  9. #79
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    Re: The Imsides method

    Hi smithy,

    Quote Originally Posted by smithy View Post
    That isn't what i said, Tilly. I was agreeing with you that calcium hydride can dry methanol, the very reason it works in the Sandy Brae, producing Hydrogen. I didn't mention anything about Calciom Oxide in the S/B.
    You are correct, I see my mistake.



    Just because Graydon doesn't mention anything in the S/B instructions about methanol doesn't mean it won't work. It does work accurately to evaluate the water content of methanol. I have had conversations with Graydon who agrees with me.
    You seem confused. I do not think of Graydon as an authority on anything and have no idea what he might or might not claim for the Sandy Brae test kit.
    I went to the Sandy Brae site to see what they claim for their test kit and methanol was not mentioned.




    It is the Carbide Manometer (updated by your mate IMB) that is incapable of measuring water in methanol.
    I remember him! he is the fellow I helped sort out one of the design problems with his reactor.

  10. #80
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    Re: The Imsides method

    I'm sure IMB was pleased with your advice.

    BTW well done with the tests. When you threw down the gauntlet to Dr Mark it was a mistake for him to claim that you would get separation on the 15gm/15titration process. Lets face it, no way on Gods earth would that ratio of chemicals have worked. Even with dry methoxide the neutralisation would produce something in the region of 0.5% water.

    However, using his drying method in conjunction with glycerol pre treated oil which shows no titration and a water level of around 350ppm gives a greater yield, plus one other advantage which is the process gives rise to liquid glycerol (good for pre treating) whereas using the liquid catalyst ASM gives rise to glycerol that sets like a brick.

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