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Made a nice batch of gel! :(
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Well I finally got my processor thawed out and running again this past weekend!
I had some oil that was sitting in my settling drum since last fall that titrated at 3 NaoH giving a total of 8 grams per liter for my my 100L batch (this is a high titration for me), I use 22% methanol.
Well this batch would not pass the 3/27 by 2AM so I let her go all night just to find the same 3/27 failure in the morning. Booo...
So I did some searching and found Tilly's reprocess recipe of 50Ml and 1.5g per liter and like an idiot I just went for it on the whole batch instead of trying a 1 liter test batch! (that has now been chalked up to experience)Frown
So everything was looking good with the reprocess and after about 2h it passed the 3/27 with flying colours so I let it settle for 24 hours. I Drained the minimal amount of glycerin and started the demething, here is where things started to go wrong.
After about an hour of bringing the bio up to temp with only minimal vac applied (5 to 10Hg) I noticed what looked like a small amount of bio colouring mixed in with the methanol dripping into my carboy of which I never gave much though to and started ramping up the vacuum for recovery, everything was working like usual except for the bio colouring I saw... That will be an indicator if this happens again!
Anyways, to make an already long story short, when I drained the bio into my new 15mic sock filter I noticed it was immediately filling up... The bio had turned to gel! After much work I got all the gel out of the reactor into my drum and went to bed. When I looked at it tonight it appears that allot of the bio has returned to liquid with a large thick coating of what looks like soap on top with liquid under it, not sure what it is like at the bottom of the drum... This goo is likely free of most of the methanol but I am not sure as the gel foamed into my methanol collection container filling it with gel and methanol...
I do not have water in the shed yet as I use the GL settling method, my question is can I recover this batch without water, or even with water?
I don't want to mess with it until I hear from some people who have dealt with this before...

I found this interesting post by Tilly about purposely making gel to indicate the completeness of the reaction, this must have been previous to the 3/27? This post makes me think that my reaction was very close and the 1.5 grams of NaoH was over the top and made it gel up?

Any input would be appreciated!
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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Hello Jon,
It is actually Neutral's reprocess formula and if you use NaOH it should be 1g NaOH per litre of oil.
Anyway, What you have is soap.
Before Tilly posted his development work on the Warnqvest Conversion test that almost everyone now seems to use to check conversion, the standard test for Conversion completion was another test that Tilly had developed. The World Famous Dr Pepper ASTM Reprocess Technique (Pat Pend) Revised which counts on high conversion biodiesel forming a soap gel within 5 minutes when it is reprocessed. So it seems your biodiesel was pretty high conversion before being reprocessed.

Water washing will cure this problem. To test put a small amount of the gel in a pan, add warm water and stir gently
 
Registered: April 03, 2009Reply With QuoteReport This Post
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Hi Riccardo,

quote:
It is actually Neutral's reprocess formula and if you use NaOH it should be 1g NaOH per litre of oil.

DOH!
Thanks for the suggestions!
I wonder if I just let it sit if the soap will settle out do to the fact that I have extracted the methanol? I am going away till Friday night so it will have to sit till then anyways...

Do you know what makes all the soap? Is it the extra caustic reacting with the glycerin that makes all the soap or the biodiesel?
Its quite the stuff anyways! Big Grin Sure took me by surprise.... Big Grin
thanks,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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Hello Jon
I have never seen a soap gel break on it's own. This is the exact reason I would Never used biodiesel that was not water washed if it were made using NaOH.
As I recall, the theory seemed to be that it is turning biodiesel into soap.






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post
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Hi Tilly,

Nice to see you!

Good info on NaOH fuel/soap gels. With all the waterless "washing" going on, this is timely.


Andrew

http://biodieselcommunity.org
03 Dodge 2500 B100 homebrew
79 Rabbit B100 homebrew
 
Location: Northern California | Registered: February 27, 2006Reply With QuoteReport This Post
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I used to use a 100 lb. propane cylinder for my reaction vessel and had no problems making bio , then i went to cone-bottomed 55 gal. drum and my first batch was ALL want I thought was glycerin.A real bummer to clean-up. It was also the first batch that I made using wvo from the bottom of a 300 gal tote. The only way to get the oil was from the bottom valve,so I think it was from water. I didn't dewater my wvo back than . Now I'm going to stir the whole tote up first by using a pump or compressed air to churn it up. I think drawing the wvo off the top will just prolong the problem.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post



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Tilly does this mean that you would use bio if it were made with KOH and only bubble washed?
The reason i ask is you americans seem to water wash a lot, i process using KOH then only bubble wash here in oz, maybe ambient temperature related i dont know. I heat to around 60-70 celsius and bubble while spray pump as well then leave it to settle for a few days all the soap drops out leaving clear bio filter it to 0.5 micron into clear carboloys then use it. I do the 3/27 shakem and soap test which pass may need to do the freeze thaw. kind regards andy
 
Location: south australia | Registered: November 17, 2008Reply With QuoteReport This Post
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quote:
Originally posted by gilfish:
. . . you americans seem to water wash a lot, . . . I heat to around 60-70 celsius and bubble while spray pump . . . .



Andy,

What do you bubble through your biodiesel; air? To me, "bubble' implies "bubble wash" which involves water.


Tilly,

Welcome back. Good to see you are back to posting. There was a time when you didn't post for a while that I thought something bad may have happened to you that rendered you unable to post. Truly, that thought saddened me.
 
Location: Illinois | Registered: February 21, 2006Reply With QuoteReport This Post
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quote:
Originally posted by gilfish:
Tilly does this mean that you would use bio if it were made with KOH and only bubble washed?
Yes if you mean bubbling air through the biodiesel.

Producer, thank you for your kind thoughts.






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post
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quote:
I wonder if I just let it sit if the soap will settle out do to the fact that I have extracted the methanol? I am going away till Friday night so it will have to sit till then anyways...


I have had thin layers of gel (soap) on the surface of a couple of my batches, prior to de-mething it. I used a kitchen strainer to scoop the majority of it off prior to washing. It could likely be washed out without doing this, but I would worry about creating an emulsion... which is a pain to clean up too.
 
Location: Winnipeg, MB | Registered: July 31, 2008Reply With QuoteReport This Post
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Hello Tilly,
Nice to see your back!
How was the cruise? I was worried you may have become another "overboard" statistic! Wink

quote:
This is the exact reason I would Never used biodiesel that was not water washed if it were made using NaOH.

That statement is worrisome to me! All the biodiesel I make is with NaoH and I just remove the methanol and settle ala the GL method, I have never water washed...
Can you elaborate on your concerns/experience with this method?
Thanks for your input,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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quote:
I have had thin layers of gel (soap) on the surface of a couple of my batches, prior to de-mething it. I used a kitchen strainer to scoop the majority of it off prior to washing. It could likely be washed out without doing this, but I would worry about creating an emulsion... which is a pain to clean up too.

This is normal, I believe it is soap left behind as the methanol evaporates off the top, it will settle with the rest of the soap in time...
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post



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Hello Jon,
I have been in India lately flat out helping my Conjoined Twin brother running our Official "Made in Australia" tourist souveniers factory.

My experience with biodiesel made with NaOH is that there is always some soap gel present. The soap gel I am talking about is a clear gel that binds the biodiesel together and looks exactly like jello biodiesel. So I always wash the soap out when using NaOH.






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post
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Producer, yes i just bubble air through it using twin outlet aquarium on full. Also use sureflo 12v pump draws off 10' above the bottom of 44 gal drum and sprays back in the top. I do it aggressively from the start, if it is only finished reactor temp 40-45C it will create 2-3' foam on top if temps are high 50-70 then no foam all done in 24 hrs. Just doesn't seem right to add water to a process that appears to hate it. i am only a newb and could be horribly wrong.

Tilly, yes bubbling air only, I see soap after methanol begins to evaporate, when i remove the glycerol from the reactor{ base/base 80/20} I put it aside in a frytol drum it is just black the next day it will have 1' or so biodiesel on top of 1/2" of white soap then black glycerol the remainder. This is also what layers on the bottom of my bubble/dry tank 44 gal drum. I have collected this dirty white soap put it in a drum put in some 98% sulfuric acid it went a dirty yellow then threw it into some fresh glycerol from a recent reaction and over a couple days 3-4" bio thanks andy
 
Location: south australia | Registered: November 17, 2008Reply With QuoteReport This Post
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quote:
My experience with biodiesel made with NaOH is that there is always some soap gel present. The soap gel I am talking about is a clear gel that binds the biodiesel together and looks exactly like jello biodiesel. So I always wash the soap out when using NaOH.

Interesting!
I have never witnessed the gel until this last batch. I suppose that a soap titration will indicate the gel as well as dissolved soaps in the bio? I need to get set up for the soap titrating ASAP!
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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Update;
Well after 3 weeks of nonstop traveling I finally had the chance to get back out my processor. Big Grin
The gel cleared! It seems that after sitting for 3 weeks demethed the gel vanished leaving behind a LARGE amount of regular white soap mixed with biodiesel. After letting gravity drain the bio sans soap into another drum the bio looks great as you can see below. I am on the road again and wont have the soap titration setup ready until next week, I will post the soap content then...
Jon



 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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Crown Royal glass ; nice touch.
With that much soap you probably had wet oil to start with.



** Biodiesel Glycerine Soap - The Guide
- on 5 continents helping people make & sell soap from the Biodiesel Glycerine.


 
Location: :-) Great White North eh ? | Registered: December 10, 2004Reply With QuoteReport This Post
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quote:
Originally posted by Legal Eagle:
Crown Royal glass ; nice touch.
With that much soap you probably had wet oil to start with.

Ya, I am not really a fan of CR but it is a nice glass. I am more of a Gibsons Finest or Alberta Premium when it comes to rye, for the last year or so I have been drinking the Irish whiskey, Jameson on ice... Mmmm... Dont even get me started on single malt scotches Smile
The oil may have been wet but I doubt it as I vacuum dry it right in the processor before I process and my oil is typically quite dry.
Too bad I didn't get a picture of it the night I drained it from the processor, it was like a big barrel of clear jello...
I am sure it was because of me screwing up the reprocess recipe by adding too much NaoH to a batch that just barley failed the 3/27... Next time I will know better! Wink
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post



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Jon

-you get my vote, TOO much NaoH been there done that(now I use KOH) never have to worry about the glop Smile Tom


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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Well to make a long story short;
I had a 1200KM road trip to make and I had less fuel in storage then I thought so I thought I would give this gelled batch a shake em up test to see how soapy it was after settling for less then a week.

That was after settling the test for about 45 minutes. A slight bit of soap cloud in the water (soft water) and no emulsion! Smile
Good enough for my old Ford 6.9 IDI! I mixed in about 60L of this into my travel tanks with the rest of my finished biodiesel and burnt it all on the road trip trouble free with no plugged filters or other noticeable problems. Big Grin Man what a nice feeling to pull into a highway gas bar and fill up the old beast in the parking lot with my own fuel instead of at the pumps for 95.9/L for their ULSD crap! Wink

So to recap;
A gel caused by using too much NaoH in a reprocess WILL settle out in time if the batch has been demethed. A slow method of decanting the bio out of all the soap is required and the bio that remains appears to be as good as the rest that I have made!
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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