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Thread: washing with heat

  1. #41
    Join Date
    Apr 2011
    Location
    Lismore NSW
    Posts
    341

    Re: washing with heat

    Hi Cade,

    looks like you're on to something here,

    I usually wash once using about 60 ltr for a batch of 1000ltrs, but my brew is kept at 65 deg at all times. after I drain the soap/water the fuel is absolutely crystal clear, even once cold. I might try to heat that to 180 deg and see what happens.

    I have a glass 2 ltr Erlenmeyer flask and give that shot. That would rule out contamination of a metal pans.

    Does anyone think it would be a issue using the flask at that temperature?

    Thanks guys
    1990 Toyota Hilux LN106 with ATG 2 tank system (sold after running 150.000 ks on mainly WVO)
    1993 Toyota 75 Series with 1 HZ engine both 75l factory tanks and a custom 170l under tray tank.
    200.000km 80% on bio 10% on WVO 10% on dino,

    "him who never made a mistake, made no discovery either"


  2. #42
    Join Date
    Sep 2009
    Location
    Brisbane (North Side)
    Posts
    740

    Re: washing with heat

    Hey Jens,

    do you mist and bubble or do you just jam in the water and belt it up with your brewer? it is interesting that you keep it heated.

    the things that really surprised me about the heating of the bio was that the 'floaties' suddenly appeared out of an otherwise pretty clear brew, and once left to cool and settle and the floaties were filtered out, that there is some drop out in the bottom of the flask. I cant help but wonder if 'floaties' plus 'dropout' = the goodies that washing removes. I will try to put some more time aside one night after work to see what happens if I wash a batch of heated fuel.

    I was thinking Tony that I could put a pyro glass (old coffee plunger) in a pan on the bbq and heat the fuel up in that. I am not sure that the metal of the saucepan is the issue, but it would be nice to know if the floaties can be made to appear before the fuel goes brown. either way I am kind of steering away from it all now, just because of the inherent dangers of 200 litres of very hot fuel just waiting to accept a flame / spark. When I first started this train of thought I wasnt expecting such high temperatures to be needed. I was kind of hoping it would all happen somewhere around 70 degrees as the methanol was removed. and maybe it will if I keep it at 70 deg for longer?? hmm? but first things first, I need to know if what I have done by heating the fuel is a positive or a negative.
    Regards,

    Cade.

    2006 Landcruiser HDJ100 (1HD-FTE) 20,000 on bio
    2006 Ford Courier(WLT Motor), 10,000 on bio
    2002 Landcruiser HZJ105r (1HZ motor) 250,000 on bio (sold)
    2006 Mazda B2500 (WLT motor) 80,000 on bio (sold)



  3. #43
    Join Date
    Oct 2011
    Location
    Perth
    Posts
    205

    Re: washing with heat

    Quote Originally Posted by Captaincademan View Post
    Well I decided to revive my train of thought on this one. I thought I would push the boundaries a little with the temperature, and found something very interesting (to me anyway).

    I put 100ml of unwashed freshly batched bio in a saucepan and put it on my bbq wok burner. heres what i noticed:

    * at around 60 degrees or so, there was visible vapour starting. no surprises - I would assume its the methanol leaving the brew.
    * approaching 100 degrees the edges of the fuel started to boil here and there - ever so tiny little bubbles. also no surprises there - just the water left over from the reaction leaving town.
    * now it starts to get interesting. the fuel started showing ripples under the surface (you could see them as the light was refracting differently) and they sort of woft around. they remained present the whole time from then on.
    * somewhere around 130 degrees (hard to tell as the temperature of the pan fluctuated big time depending on where in the pan I took my reading) it started to change colour slightly.
    * somewhere between 150 and 180 degrees it went a nice treacle brown. heating stopped at this point.

    now its even more interesting - there are a heap of floaties that are in suspension all through the fuel, and its that lovely treacle brown colour. I then took this heated fuel and put 20ml of water in it - applied with a hand pump sprayer on fine mist - and let to settle. I did a second one with non heated fuel to compare.

    So I wanted to see this process again, so I repeated and got the same results. I ran this fuel while it was hot through a 2 micron filter and the clarity was exceptional. I left this to cool on its own.

    I repeated a third time and viola, around 180 degrees it goes brown and floaties appear. I cooled this one in some ice water to get it back to room temp, and the floaties remained in suspension. I then filtered it, and once again the clarity was exceptional. I left all of this over night. note - I also filtered some un heated fresh bio to compare - and the clarity was also very good.

    next day, the washed fuel samples are starting to clear, and as expected are not completely washed, so they are not very clear.

    both of the heated samples - cold filtered and hot filtered are showning some drop out, which is not present in the un heated control.

    the cold filtered fuel is crazy clear. when I put a LED torch under it and shine it up through it, you would expect to see a shaft of light, but you dont, as there is nothing in suspension to pick up the light. very impressed. The next little experiment will to be do a wash on it and see if it is any different to the first heated but unfiltered washed sample.

    so if the heating does appear to perform the same function as washing, I am thinking of making the following rig:

    build a turk burner outside my shed, and plumb a copper line from the bio brewer to it with a small 12v pump on the cold side with a bypass and valve so I can regulate the flow. Pass the fuel through the turk burner in a copper coil, and then send back to the tank. install a digital temp gauge to monitor the output temp. I should be able to regulate the temp by adjusting the flow. find someway of working out the flow rate and then try to make this predictable at each batch so i can then just run the pump for a period of time, allowing for say 3 changes of tank volume.

    after this its just a case of running off any sediment and filtering the fuel. I reason that the sediment should drop out regardless of filtering, I just filter it on the way to the storage tank after it has settled for a few days.

    My only concern is what have I actually done to the fuel by heating it to 180 degrees? is the brown colour caused by carbon or something such as? have I 'burnt' the fuel and reduced its calorific value?

    I am looking forward to hearing some comments - good and bad on what I have done or what I could improve, or if the process has no value at all.
    The brown stuff is caused by the methyl ester polymerising. As it's unsaturated it's prone to this, and is promoted by heat (as it readily exceeds the otherwise substantial activation energy of the process). But in a broader sense (as I've attempted to explain before) the problem with this approach is azeotropes. In simplest terms, if you have a mixture of liquids, one doesn't necessarily start to boil off when you reach its boiling point. And methanol is prone to this more than most chemicals due to its small size and propensity to hydrogen-bond with other organic molecules. https://www.drchemical.com.au/uncategorised/biodiesel

  4. #44
    Join Date
    Sep 2009
    Location
    Brisbane (North Side)
    Posts
    740

    Re: washing with heat

    Hi Mark,

    The floaties do not appear to be brown. they appear to be a whispy whitish. they are the same density as the body of the fuel, i.e. they do not sink or swim. they stay suspended nicely. the total body of the liquid changes to a brown hue, completely evenly distributed. there is a slight amount of brown dropout that appears on the bottom after a few hours though, looks exactly like glycerine sitting in the bottom. intersetingly the sample that was hot filtered had more dropout than the sample that was cold filtered.

    interesting point about the components not boiling off at their respective temperatures. dont forget Mark, a lot of us are not classically educated and our eyes glaze over with use of terms we are completely unfamiliar with - such as 'azeotropes'. we sometimes need a lay explanation to assist (as you have done so in the post above - thankyou).

    given your access to good gear and a scientific approach, would you mind please heating up some unwashed bio (made with a single stage method) to around 180 degrees and putting some comments on as to what you observe? I know this is putting you out, and completely understand if you dont have the time or inclination, but I'm sure the broader community would benefit from the experiment being done properly rather than done on a greasy old bbq outside in the wind with more variables than you can imagine.

    I will still persist as I am pretty keen to see where this goes, and whether or not there is a process that can be developed which is safe and efficient..
    Regards,

    Cade.

    2006 Landcruiser HDJ100 (1HD-FTE) 20,000 on bio
    2006 Ford Courier(WLT Motor), 10,000 on bio
    2002 Landcruiser HZJ105r (1HZ motor) 250,000 on bio (sold)
    2006 Mazda B2500 (WLT motor) 80,000 on bio (sold)



  5. #45
    Join Date
    Nov 2005
    Location
    Tasmania
    Posts
    523

    Re: washing with heat

    G'day Cade, this may not be relevant in this case, but may add some light to what's happening. Have only ever heated BD when drying on the sun, but have heated VO to almost boiling temp to see what happens to the oil. Have seen those white floaties when it goes over 200deg C and wondered what they were, when the temp goes over 210degC, they disappeared. Have also found when the VO is heated over 206degC, it turns a bit brown, almost like it is burnt. It really thins the oil and stays that way and there is a lot of fatty stuff in the bottom when it cools down. Some one told me it wasn't fats, but some other stuff which should be removed during the oil processing, it might have been silicate or something similar and is in the fibre of the seed.

    I tried the heating method to see if it made it easier to work with and it did, but the centrifuge does the job with a huge reduction in labour and time, stopped doing that. It was a bit dangerous when the oil started to evaporate above 216degC. When I make BD again in a couple of months, will heat it up to see the results and let you know if you haven't work it out by then.

    Agree with you about the technical jargon, loses me. I'm a think about it, work out the plan, safety levels, then experiment to see if it works and what happens.

  6. #46
    Join Date
    Sep 2009
    Location
    Brisbane (North Side)
    Posts
    740

    Re: washing with heat

    Hi Alga,

    sounds like you have observed something pretty similar to me with the brown colour and floaties. interesting that they disappeared??? (key in spooky music)....

    Hey Jens - sorry I didnt read your post properly, if you want to jump in on the action would love you to try and repeat and perhaps get a better result, particuarly if you have better equipment than I (which isnt hard mind you).

    Just a word of caution to anyone heating up bio, once it reaches its temperature of around 130 degrees it will accept a flame and ignite, which is quite different to its normal benign properties at room temp.
    Regards,

    Cade.

    2006 Landcruiser HDJ100 (1HD-FTE) 20,000 on bio
    2006 Ford Courier(WLT Motor), 10,000 on bio
    2002 Landcruiser HZJ105r (1HZ motor) 250,000 on bio (sold)
    2006 Mazda B2500 (WLT motor) 80,000 on bio (sold)



  7. #47
    Join Date
    Apr 2011
    Location
    Lismore NSW
    Posts
    341

    Re: washing with heat

    Quote Originally Posted by Captaincademan View Post
    Hey Jens,

    do you mist and bubble or do you just jam in the water and belt it up with your brewer? it is interesting that you keep it heated. .
    Hi Cade,

    I have a 3/4 inch metal garden sprayer from bunnings mounted upside down in the processor. In terms of misting, that's how fine it gets.

    I add 50ltrs of water to the mix with the methoxide still in the brew as a pre-wash. Once the methanol and glycerin has been removed, I add another 50 or 60ltr to the bio and turn the paddle mixer on for 15 min or so.
    I the let it all sit for a couple of days and drain the water/ soap out and run the bubbler until the bio becomes crystal clear.

    With the brew staying warm everything settles out a lot easier and no emulsion is formed I find. Mind you all my bio gear is running off our off grid solar system, so power costs / consumption is of no concern.

    All up it can take up to 5 days per batch of bio, but since I am making 1000ltr at a time, I have plenty of bio in storage so time is not an issue either.

    I'll see that I get a chance to have a play in the next few weeks and get back to you.

    Have fun!
    1990 Toyota Hilux LN106 with ATG 2 tank system (sold after running 150.000 ks on mainly WVO)
    1993 Toyota 75 Series with 1 HZ engine both 75l factory tanks and a custom 170l under tray tank.
    200.000km 80% on bio 10% on WVO 10% on dino,

    "him who never made a mistake, made no discovery either"


  8. #48
    Join Date
    Oct 2011
    Location
    Perth
    Posts
    205

    Re: washing with heat

    Quote Originally Posted by Captaincademan View Post
    Hi Mark,

    The floaties do not appear to be brown. they appear to be a whispy whitish. they are the same density as the body of the fuel, i.e. they do not sink or swim. they stay suspended nicely. the total body of the liquid changes to a brown hue, completely evenly distributed. there is a slight amount of brown dropout that appears on the bottom after a few hours though, looks exactly like glycerine sitting in the bottom. intersetingly the sample that was hot filtered had more dropout than the sample that was cold filtered.

    interesting point about the components not boiling off at their respective temperatures. dont forget Mark, a lot of us are not classically educated and our eyes glaze over with use of terms we are completely unfamiliar with - such as 'azeotropes'. we sometimes need a lay explanation to assist (as you have done so in the post above - thankyou).

    given your access to good gear and a scientific approach, would you mind please heating up some unwashed bio (made with a single stage method) to around 180 degrees and putting some comments on as to what you observe? I know this is putting you out, and completely understand if you dont have the time or inclination, but I'm sure the broader community would benefit from the experiment being done properly rather than done on a greasy old bbq outside in the wind with more variables than you can imagine.

    I will still persist as I am pretty keen to see where this goes, and whether or not there is a process that can be developed which is safe and efficient..

    I’m sorry but I don’t have access to the facilities for this. It’s a job for a GCMS and I don’t happen to have one of those floating around.
    Also, unlike some people on this site I’m not going to guess and then act as though I know what I’m talking about
    Last edited by Dr Mark; 30th January 2019 at 07:27 PM.

  9. #49
    Join Date
    Jan 2006
    Location
    ลึก ประเทศอินเด&
    Posts
    2,061

    Re: washing with heat

    Hi Mark,

    I’m sorry but I don’t have access to the facilities for this. It’s a job for a GCMS and I don’t happen to have one of those floating around.
    Also, unlike some people on this site I’m not going to guess and then act as though I know what I’m talking about
    I am so glad to see that you finally realize it is necessary to perform the testing BEFORE you post the test results.
    I assume you will now be changing the misinformation you have repeatedly posted to this forum claiming that the standard single stage Base method can not produce biodiesel at room temperature.


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