Hello.
I've been making 34 gallon batches with KOH in this first year of producing bio.
I have had success in processing 2 stage reactions 80/20 90/10 formula.

I have standpipe mistwashing and drying tanks. Now clean and dry as new for settling/post treatment.
I have a 4"x57" Steel resin column I built and a #2 bag filter pod w/5 micron filter bags.
Purolite PD206.



Friday, I did my first 34 gallon batch with NaOH 99%pp.
The oil was settled, clean and dry and pretreated with raw glycerin- as all of my batches are.
The titration was 1g over base (5g/l) This stuff wants to be biodiesel.
5/45 Varnquist test was clear and no fallout. Yellow tint as usual.
Had an 'IP' test at the plant and bound glyc was .1. So onward we go.

I did a writeup on here about bubble demething/soap drop with KOH- no heat.
It worked great, took a week or so. But I think doing this with sodium will produce gel throughout.
It did on the benchtop with heat.

So, how is settling NaOH different from KOH?

Last night, I ran it @ 150*F for a while to drive some methanol out the vent.
Didnt work so good -no condenser.
I put it into the SP wash tank and placed a fan over it.
This morning, there is the soap skim on top, which I expected.



IF I did this method to demeth, and WHEN I get it to gel, would sending it back into the processor cold along with 2 gallons of the 7gal I reclaim of Saint Glycerol to liberate the soap/gel do me any good? Or would it effect my reaction?

This ~2 gallons of glycerin is from the second stage, mostly.
The first ~5 from stage 1 is kept for pretreatment.

I'm not pressed for time, though fuel prices are starting to get stupid again.
But I am about to try a batch of my new Chinese food WVO, ASAP.

I have a completed pvc woodchip column, but only about a pailful of red oak and no source for more.



I need to know what most folks are doing at the stage I'm at without condensing.
I have a feeling that 'plumber's delight' will come up.
I never built one.
I do have a radiator with a AC condenser from a minivan. it has a 12v fan attached. To add to this I have a toy train-set rheostat that converts 120v to 12v. Just need a design strategy.

I also have a dozen clean, open top drums w/ringlids and one available 330 gallon IBC tote.

Shoot me some experience, guys.

Brian

Brian,

I am not sure what your asking.

You could send it back into the processor without the glycerine and heat again to 150 plus degrees. That should flash off some more methanol when you transfer it to the settling tank. You could just bubble it for a day and wait a few days to run it through the wood chips. My last stuff that I used in the truck didn't even need to go through the wood chips. It had settled for about 3 weeks though. I ran it through the resin column because I had it. There was actually very little soap to drop out of that batch. Very good conversion.

Thanks, Eurocab.
Quick reply.

Today, I turned the heat element on and have been stirring it with a sledge hammer handle once in a while.

I have a sample on my hot plate (bottom half of a Mr. Coffee), doing the same thing.
Seems to be working ok. Tiny bubbles and clear soap on the bottom. Thin skin on top.

Will the top skin drop over the 3 weeks, or do you skim it off?
I dont recall the top skin with KOH. It does fall or seems to when I stir it.

I'll try the bubbler, I just hope it all falls below the SP.
I'll hang the bubbler above the presumed level of drop out to disperse the heat.

Wow, three weeks, I'll put it in drums after the demeth so's I can move along.

Thanks.
Brian

I could not find a steady source of wood chips, so I dont even want to experiment with a full batch.
I need a standard operating procedure.

Brian

quote:

Will the top skin drop over the 3 weeks, or do you skim it off?

Yeah the skin is soap and it will settle to the bottom. I usually break the skin up when I see it. That allows additional methanol laden BD to get surface air from a fan. I think bubbling is a fairly fast method to drive off the methanol. Some are afraid that it might polymerize the BD. It hasn't been my experience.

The nice thing about NaOH is settling out the soap and the cost savings.

quote:

Some are afraid that it might polymerize the BD

This is why I'm refraining from recirculating in the heated dry tank.
That, and oxidizing.

I use airtool filters, so I have big gentle bubbles. It moves the heat well, too.



So I put it on and it's going now. all seems well.
My sample is also flashing away in the same manner, but no bubbler, just an occasional swizzle with the thermometer.

I'll keep breaking up the skin with the whoopin' stick.

Thanks for bein there.
much help = more confident.

Brian

quote:

But I think doing this with sodium will produce gel throughout.
It did on the benchtop with heat.

I jumped the gun on this one.

My benchtop bubbling in a 175ml was just too aggressive.
Gel was produced thru an open tubing bubbling like mad over heat.

(edit) the gel was just a rolling glob, it didnt gel the whole sample, though I have seen this in overdosed mini batches.

I think I had an acceptable conversion and Eurocab has helped me to
just go ahead and bubble the big batch. I also used a heating element and mild fan.

The new sample is almost done flashing off and there is some gel skin on top and at the bottom of the beaker is transparent soaps- very little - maybe 8ml of 175ml.

Hope this helps the drywash threads.

trust me, I'll have more inquiries in the next couple days/weeks.

Brian

Graham Laming demonstrated with his GL Eco System that using NaOH as the catalyst that the soaps that are in suspension will drop out of solution when the methanol is removed from the solution. Ergo; a method of circulating and heating the settled biodiesel minus it's glycerine layer to methanol's evaporation temps (148.5F) + a little and recovering it via condensing coil will have as it's effect to settle whatever soaps might have been left in solution to settle on the drum's floor.

Based upon this I designed my system which uses a separate settling drum immediately after reaction equipped with a standpipe to drain off the settled biodiesel first and leave the glyc layer behind.

GC testing has shown that I am getting an ASTM passing grade of 0.240 total glycerine, and this just from settling a couple days.

Passsing it then through a lead/lag resin bed configuration gives me an ASTM grade of 0.161 minutes later, a 30% reduction from resin purification on a product that was already good to start with.

Hard wood chips are showing great promise; after settling the numbers are impressive. A start point of 800ppm going in on a single pass gives a zero for soap coming out, so IMO, the best of both wolrd's is to use separate settling drums, demeth the biodiesel and allow soaps to drop out of solution and then run the settled BD through a hrad wood chip tank followed by lead/lag resin tanks.

I final polish using a CAT canister fuel filter down to 2 microns. I have biodiesel thath has sat for several months and there is no dropout to be seen anywhere. The only water I ever use is recycled for the methanol recovery condenser; I use none for the biodiesel production side

HTH

I demeth via bubbles for ~12 hrs then settle for a week. The last batch had a soap ppm of 274 after demeth and settling. I utilize a higher end aquium pump and two brass pneumatic mufflers on a brass T for bubble stones.

quote:

Passsing it then through a lead/lag resin bed configuration gives me an ASTM grade of 0.161 minutes later, a 30% reduction from resin purification on a product that was already good to start with.

LE,
Thanks for checking in, I refer to your website often.
Culligan never got back to me about picking up old water softener filters.
I wanted the same system as yours.

As for the quote;
I didnt know resin would lower the TG. The Free Glycerin however, can be reduced by washing wet or dry.

I've considered settling the whole batch, glycerin and all in it's own drum.
I do the glycerin pretreatment, so I drain 5 gallons into a #2 poly chemical cubie from the processor and seal it.

I drain about another gallon + and a skim of bio, then transfer to the SP wash tank via processor pump. I know some residual glycerin gets to the washtank/settling tank.

I have searched high and low for hardwood chips. I had been following postings about the process for months.
I just cant find a steady source to commit to it. My son in law has a wood chipper, but that's pretty labor intensive and another mess to clean up. I only process about 68 gallons per month.
More than I can use.

I also refer to GL's website.
I dont do the 5% prewash. My new process has not used a drop of water.

I want another settling tank if soaps take weeks ro fall out after demething.

I have found a used 250 gallon poly tank that is tall cylindrical shaped.
I'll post a new subject about mixing/settling multiple batches in one tank.
This would save a huge amount of space in the shop.

Brian

quote:

Originally posted by dckfly:
I demeth via bubbles for ~12 hrs then settle for a week. The last batch had a soap ppm of 274 after demeth and settling. I utilize a higher end aquium pump and two brass pneumatic mufflers on a brass T for bubble stones.

Hi dckfly,
What is your batch size?
I have the same brass bubbler stones as you (see pic above) on a $5 aquarium pump.

Do you use heat?
I hang the bubbler near the hardwired heating element low but not on the bottom of the drum
This moves the heat very well.

I've gotten it up 150F and kill the heat and continue bubbling for 3 days, now.

I dont know how much methanol is left. I heated a beaker up to 150+F and no bubbles
from methanol arose.

I now have globs of soap swimming around and the reoccurring frothy top skin.
I assume from GL's site that this is to be expected.

I will stop the bubbler today, clean the snot from the heater and bubbler, test for methanol and let it settle.

I will order the soap titration kit to do this right.

Thank you for your input.

Brian

By the time got home the skin was all gone.

quote:

What is your batch size?
I have the same brass bubbler stones as you (see pic above) on a $5 aquarium pump.

Do you use heat?
I hang the bubbler near the hardwired heating element low but not on the bottom of the drum
This moves the heat very well.

I do 152L batches in a 209L steel drum. I just started this process (pre-wash, demeth, chips) this summer so there is enough natural heat, about 15-20C, that heat does not seem to be necessary right now. Come winter, though, I will need to add some heat, how much I'm not sure yet. It will take some trial and error. We also have the advantage of a dryer climate here in Boulder than you do in Indiana which may help quite a bit. Winter here is evern dryer than summer so I suspect that I will only have to add enough heat to keep it at about 15 - 20C range since it seems work now. Winter here is actually fairly mild, usually, so there is only about a month or two that trying to fight the elements to brew just isn't worth it.

You might also consider implementing a 5% pre-wash since this seems to pull a large amount of soup, unused catalyst, etc. from your raw BD.

Hope this helps

quote:

You might also consider implementing a 5% pre-wash since this seems to pull a large amount of soup, unused catalyst, etc. from your raw BD.

Thanks,
I have considered this, and with it's popularity, I probly will end up trying this.
This batch, I was trying to mimic LE's waterless system.

I've done several different processes this year to find what I'll be comfortable with.
I have the advantage of having more good oil than I can use.
My fuel consumption is minimal- maybe 50 gallons a month at most.
So I can experiment with different things and not be press for a tank of fuel.

In the mean time, I'm enjoying designing and building my 'mega seed' processor.
It's a re-fabbed 66gal electric water heater with ~100gpm pump.
It will have condensing capabilities and an eductor.
http://biodieselpictures.com/viewtopic.php?t=669

It's day five of settling, I'll do some testing today.

Brian

Estimates indicate and my experience thus far confirms that the pre-wash removes about a 1000ppm of soap from your raw BD.

Checked out your pics - your new rig looks sweet! I also am quite envious of your work space. I would kill for that much room. I do everything in a single car garage! What do you do for a living and what are all the large silos in back ground?

Dana,

I'm going for it. I got a batch of my new Chinese buffet oil settling glycerin pretreat.
Friday I will pull the glycerin and react it 80/20. It will be a 3% pre-water wash.

I did a search and read about the 2 stage process using prewash for those who want to retain raw glyc for pretreatment.

This will bring up more settling questions.
This water will need to dried out. I guess I can dry it in the original drying tank.
That uses heat and circulation spraying. An other thing I was trying to avoid. But I feel it should go quicker than a mist wash drying.

Oof, I also have just a 1.5 car garage. Since I closed my shop, I can hardly walk in there.
I also have my daughter's garage full of steel and a 2 axle trailer full of stuff I wont part with.
Those pictures are from when I was welding at the new local BD plant last winter.
They have become great friends and are very helpful to my homebrewing, such as glycerin disposal and QTA testing. I'm considering working there myself. I go hunting with guys in management and have been invited to sign on.
In one picture you see my catwalk, 30,000 gal settling tank and 3 'fuges.
the stainless tanks are pretreat system.

I have samples of the Chinese buffet oil pre and post glycerin scrubb.
I'll HPT the samples. Or QTA if I get up there this week.

The current batch, 6 days settling, will have to go to a steel open top drum via SP. I guess for 2 more weeks. I'll clean the tank of soap for observation of the difference.

So do I send it to bubble/settling first or dry/demeth it in the dryer first?
Seems either way will work, but the dryer makes more sence. I'd need to open up the whole shop and ventilize the room, or wheel it outside.

I'll get a soap titration kit in a couple weeks. I'm recouping from school supplies and clothes.

Brian

Once the bio is properly demethed any soap will soon drop out, KOH based bio will take longer to settle out the soap than NaOH based bio does, I recover almost all of the methanol in my processor then drain the glyc and pump the bio to my settling tank where I bubble with 3.5 litre per min aquarium bubbler overnight (folks with more powerful air pumps like 60LPM + pumps only need a few hours) Then leave for soap to settle for minimum of 12hrs but usually 24hrs and filter and use.

"This will bring up more settling questions.
This water will need to dried out. I guess I can dry it in the original drying tank.
That uses heat and circulation spraying. An other thing I was trying to avoid. But I feel it should go quicker than a mist wash drying."

No need to dry water from prewash, it comes out with the byproduct and what little might remain will be taken care of by your dry filter.

quote:

No need to dry water from prewash, it comes out with the byproduct and what little might remain will be taken care of by your dry filter.

Hmm, ok...
I'm way ahead on fuel, this is when I like to experiment.

On Andrew M.'s suggestion in another thread, I'll add only a couple liters off water to the second stage glycerin. I'm contemplating adding some of the stage one glycerin and using a gallon of water.
I'm sure 3 gallons left over raw glyc from stage one would pretreat the next 130L just fine.

I qta tested the Chinese food wvo pre and post treatment.
The FFA% went from 2.2 to 0% after glycerin scrub. What's up with that?
Water% went from 0.13 to 0.03%.
Titration went from 3 to 2 ml/l Na. Shoulda been better than that?

The test was from a jar I pulled right before stopping the pump with glycerin in the oil.
I'm pulling the settled glycerin this morning and want to re-test today's oil.

I mixed at 130*F for 30 minutes, settled 1 day and 1 night.

Recap later...

Brian

Brian,

How did you test for FFA's? I have never heard of 0 FFA. The titration of 2 indicates that there is still acid present in the oil.