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KOH doesn't seem to work too well with the waterless wash process...cant get the soaps to settle out or filter out... even w/ a 5 micron bag filter.


A few of use have been talking about this quite a bit at
http://biodiesel.infopop.cc/eve/forums/a/tpc/f/719605551/m/2441007202/p/1

What I seem to know about using KOH and water less washing;
1) A 5% water prewash will make KOH soap float during the methanol removing.
2) The more violent you are blasting the BD back into the tank the more floating soap you make and the more you can skim.
3) Thicker filters catch more soap; even if its the same micron rating, you catch more soap. i.e. two 5micron filters inside each other will catch more soap than a 5 micron filter. I use a four layer 25um/10um/5um/1um as the final "polish" and get clear water in a test wash.

I have no PPM numbers to report to back up my claims yet, as I need to get some chemical bottles and mix up the solutions. Come over to the address above to read all the fun! Big Grin
 
Location: Southern WI, USA | Registered: 18 May 2006Reply With QuoteEdit or Delete MessageReport This Post
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okay, so i've now made a 100l batch using GLs process using NaOH as catalyst. distilled about 5l of methanol(and/or water) out of the batch before transferring to settling tank. started filtering and it immediately plugged up a 100/5m double layer filter setup. i'm assuming it was plugged as the pump started to struggle to push bio through the filter - and the filter was total rigid and fully expanded...and started to leak a little around the seams.

next day...

so i decided i would just let the bio recirculate for a while. about four hours later, i stopped and scooped some soap out (not a very thick or consistent layer) then put another bag filter on. saw that build up some pressure too. and the bio did not clear up at all.

so i decided i would let it settle for 24 hours. today it is no more clear than it was when i started.

it is routinely over 100 degrees here during the day (and hotter in the garage)...maybe the soaps don't like to settle when the bio stays probably over 90f all the time?


what do you all do after distillation? am i missing anything?

on edit: i did not do the 5% prewash. do any of you use the venturi to add the water, or do you use the appleseed-style methanol injection port?
 
Registered: 16 February 2006Reply With QuoteEdit or Delete MessageReport This Post
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I am surprised you got 5ml out, I have only been getting about 2 ml from a 100 ml batch.

If you can spray the demethed BD into your filtering tank and let it circulate like that or 4-8 hours you should find that some soap will clump up and float tot he top. You can skim it off at that point. Doing this will bring your soap content way down and then you can do a final bag filtering stage if needed.

I've been sparaying for 8 hours, scooping off the soap gunk from the surface, and then filtering through 5 or 1 micron filter bags for 4-6 hours and getting less than 200 ppm biodiesel from this process.
 
Registered: 10 March 2007Reply With QuoteEdit or Delete MessageReport This Post
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That should have read 200 ppm soap content in the biodiesel after filtering.
 
Registered: 10 March 2007Reply With QuoteEdit or Delete MessageReport This Post
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Hey, been following this thread for a while, first time to post.

We've tried out removing methanol from bio with the hopes of simplifying the wash process or, if all goes well as graham describes, getting rid of it. We are using chicken fat with NaOH, but after we recover the methanol our biodiesel turns into jelly! I had discovered this in the lab a few times but thought it was just a lab anomaly, but since we've found the same thing on a larger scale and I'm wondering if anyone has experienced this. It literally turns the biodiesel into jelly, it's very odd. Nothing is wrong with the bio (it passes glycerine), and has been settled overnight so should be relatively glycerine free.

The only difference I see is that we're using chicken fat, so that's my guess as to the cause. We're going to try to filter it (1 and 10 micron) immediately upon existing the methanol recovery system with the hopes that it helps. Any thoughts/theories?
 
Location: Pittsboro NC | Registered: 12 December 2006Reply With QuoteEdit or Delete MessageReport This Post
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Hi gbathree

A couple of questions for you ...

How much NaOH did you use per litre of fat?

How much methanol did you use per litre of fat?

Did you dry the fat completely before you made the bio?

What was the titration value?

------------

It sounds like you may have a lot of soap in your bio, and this could be because the fat has a lot of water and/or a lot of FFA in it, or because you are overdosing on NaOH or under-dosing on methanol, or a combination of these.

If you gently warm the bio, does the jelly liquify? If so, at what temperature does it become completely clear and liquid?


Rover 75 + Skoda Fabia on B100
http://www.graham-laming.com
Bicycle on G100 12,000 miles p.a. ( http://tinyurl.com/krppyc )
 
Location: UK | Registered: 04 December 2005Reply With QuoteEdit or Delete MessageReport This Post
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Sorry for the late response:

I used the same amount we always use which gives us ASTM spec fuel - I'd have to check and see exactly, but just trust me, it's the correct amount. Our feedstock is always below 2000 ppm moisture, so we don't have excess water - especially because we're using sodium methylate which has no water in it. Our chicken fat titrates at between 1 and 3, usually around 1.5 or so, so it's good stuff. Chicken fat is solid at room temperature, so we get it hot, store it hot, and use it hot.

I have had it jelly by: a) heating a few hundred mls in the microwave, b) heating a few hundred mls on a hot plate and c) sending 20 gallons through a flash evaporator (heat and vacuum) and recovering the methanol that way. In the 20 gallon batch, I sent the jelly bio through a pump and through a 20 micron filter, to find that it quickly clogged it. Filtration definitely gets the soaps out, but the problem is there are a lot of soaps!

Since this, we've switched to potassium methylate, and I'm going to see if instead of jelling, we will get the soaps to settle to the bottom or top of the container.

That's the news, I'll let you know how the potassium methylate recovery goes.
 
Location: Pittsboro NC | Registered: 12 December 2006Reply With QuoteEdit or Delete MessageReport This Post
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Am I the only person that does not filter their biodiesel during the waterless wash process? I simply remove as much methanol as possible in the processor recovering it. Then transfer it to my washtank where it gets bubbled for 12-24hrs ... done!!!! A sample in a jar with water - shaken ...clear water no soaps??? no skiming off the top and I use KOH ... gee either I am doing something right or I have gotten it all wrong???


HDJ80
Canberra
 
Location: Canberra | Registered: 07 August 2006Reply With QuoteEdit or Delete MessageReport This Post
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Hi HDJ80
"....Then transfer it to my washtank where it gets bubbled for 12-24hrs ... "
Washtank with or without water?
If it;s without water, then:
Why do you bubble? -to de-meth?
Do you find soap on the bottom of the washtank?
 
Registered: 13 November 2006Reply With QuoteEdit or Delete MessageReport This Post
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Hi HDL80

I don't filter my biodiesel any more. Haven't filtered in the last 6 months. I just let it settle in a covered tank and let gravity do the work.

I replace my fuel filter on the car every 5000 miles. The fuel is plenty clean enough, and the fuel filter is there to catch any bits. I cut them open after removing, and they are probably good for enother 5000 miles. Look clean to me.

Much easier, less hassle, less cost and no problems.

This is my opinion only, and it suits me fine.


Rover 75 + Skoda Fabia on B100
http://www.graham-laming.com
Bicycle on G100 12,000 miles p.a. ( http://tinyurl.com/krppyc )
 
Location: UK | Registered: 04 December 2005Reply With QuoteEdit or Delete MessageReport This Post
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Graham, Yes I forgot you gave that up. It just seems that those that have issues are all relating to removing soaps filtering them out, how messy. Yes I basically do the same except bubble air through it to remove the last of the methanol...
Yair-BHFC ... No water and basically all the soap ends up in the bottom which is drained off on it's own. The finished bio is drained from about 8" from the bottom of that tank leaving around 20litres always in the bottom. I haven't used water for 10mths or more, GL helped me out to begin with and now all is awesome...


HDJ80
Canberra


ImageBio_Plant_1.JPG (77 KB, 291 downloads) Processor setup
 
Location: Canberra | Registered: 07 August 2006Reply With QuoteEdit or Delete MessageReport This Post
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Hi gbathree

Whats your FFA level, I also use chicken fat but I had to always pretreate it to bring down the FFA to a nice level


"Learn from yesterday, live for today, hope for tomorrow. The important thing is not to stop questioning."
 
Registered: 22 July 2006Reply With QuoteEdit or Delete MessageReport This Post
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HDJ80, what is that nice 10 gallon wide mouth tank you are using for methanol? Trying to locate something larger than 5 gallon carboys ...
 
Registered: 22 August 2007Reply With QuoteEdit or Delete MessageReport This Post
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Hello All,

After much research and many hours hanging on every detail in this thread I have finally finished my processor. Well, almost, no insulation yet. The maiden voyage was last Saturday and it went off without a hitch. 150l of oil titrating at 4.5 naoh, 33l of methanol, 1425g naoh and after 4 days of settling I have about 145l of very nice looking fuel, passes 3/27 and soap is about 200ppm. Thats assuming I have the soap test right Roll Eyes I heated to 130f and injected methanol thru the venturi. It is a Mazzei 684 injector and took about 30 mi. to go in. Processed for 2 hours and tested, 3/27 was close, let it go another 30 min and it passed. 7.5l added for prewash again thru the venturi and let that run for a hour. I let it seperate for about 3 hours and could wait no longer. Drained off 35l of glycerin and went to distillation. I got about 3l of methanol at 93% in about 90 min. and in to settle it went. The pump is a grundfos 26-99 and can move 29gpm. The controller is my own and consists of a PID with 2 thermocouples. One is at the pump return for process temp. control and the other is at the condensor head for control during distillation.
It is switched so that the pump must be on for the PID to have power so no pump,no heat. The heater can be run on either 120v or 240v and is selected by plugging into one of two outlets on the bottom of the controller. Pump and heater power are fused in the controller. Condensor is a standard Plunbers Delight 4' long. The valving and gauge at the top is used when I pull vacuum or pressurize to load/unload the processor. Sorry this post is soooo long.

Thanks All (especially Graham and Jim)
Tony in Tampa


1983 Mercedes 300D
GL processor
You're not finished when you lose,
You're finished when you quit.


ImageIM000453.JPG (80 KB, 283 downloads) 60 Gallon Air Tank
 
Location: Tampa, Fl | Registered: 27 April 2007Reply With QuoteEdit or Delete MessageReport This Post
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NOW it's finished Big Grin


1983 Mercedes 300D
GL processor
You're not finished when you lose,
You're finished when you quit.


ImageIM000454.JPG (89 KB, 324 downloads)
 
Location: Tampa, Fl | Registered: 27 April 2007Reply With QuoteEdit or Delete MessageReport This Post
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Very neat Tony, well done.

Jim.
 
Location: Suffolk, UK | Registered: 08 November 2006Reply With QuoteEdit or Delete MessageReport This Post
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Thanks Jim and that venturi your sending will be the next upgrade.

Tony


1983 Mercedes 300D
GL processor
You're not finished when you lose,
You're finished when you quit.
 
Location: Tampa, Fl | Registered: 27 April 2007Reply With QuoteEdit or Delete MessageReport This Post
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quote:
Originally posted by slickhorn:
HDJ80, what is that nice 10 gallon wide mouth tank you are using for methanol? Trying to locate something larger than 5 gallon carboys ...

It is a drum used for Home Brewing Beer / Fermenter


HDJ80
Canberra


ImageMethOxide_Pickup.jpg (21 KB, 237 downloads)
 
Location: Canberra | Registered: 07 August 2006Reply With QuoteEdit or Delete MessageReport This Post
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%FFA is between 1 - 3, so it's good stuff, we don't need to pretreat.
 
Location: Pittsboro NC | Registered: 12 December 2006Reply With QuoteEdit or Delete MessageReport This Post
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Thank you Graham Laming for the undeniable amount of research and willingness to share your knowledge. . .very much appreciated and inspirational.

Has anyone attempted the "GL 1day" and equipment implied on a larger scale. . .say. . .100 - 200 Gal(400 - 800 Litre) Batches?

I am in the process of upgrading and updating my batch processing system and want to have the ability to do small scale commercial/cooperative scale production. Before I embark on fabrication and assembly, I'm trying to cover all my bases.

Thanks
 
Location: New Orleans | Registered: 28 July 2006Reply With QuoteEdit or Delete MessageReport This Post
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