Hi,
I just did a 32 liter batch of KOH Bio.
The oil was right out of my oldest cubies I had at home.- I keep my cold upflowed tote at work and wanted to clean up around the yard.

Anyway, since it was right out of the cubies, I poured each cubie into a 5 gallon bucket and only took the golden thin oil. I got a lot of food particles. I poured it into the top of the processor.

I followed this with a 130* glycerin pretreat- which is now standard practice for me even tho this source titrates around -2 NaOH.

I had the pretreated oil run on Cognis QTA and it came out .4% FFA and .03% moisture. 'Awesome!', I thought.
I didnt titrate. I wish I knew how to recipe from these percentages--any help there?
I entered the data into Rick da Tech's on-line calculator as T-2 KOH, 20% MeOH.

The 2 stage went excellent and all seems normal.
Passed Varnquist with crystal clarity.

Here is where I'm at,
While processing, I was faithfully on this forum looking for relevant discussions on KOH. This is the third type of caustic I'm trying.
I read a discussion about just setting soap and just filtering. It was from 2007-8.
I'm set up to water wash and I have my 7 gallon bag filter pod loaded with Purolite/5 micron sock.
Not sure what I want to do yet.

The discussion convinced me to transfer the bio to the standpipe wash tank and leave it bubbling cold with a fan.
Ambient temp was around 80*f.
The reaction was Saturday. Today is Tuesday. I stopped the bubbler and there is a good layer of yellowish-white soap on the bottom, none on top.
It's almost like a glycerin separation down there. I read this is normal and am quite impressed.
Had I gone strait to water wash, my first drain would probly be like shampoo.
I did 20% alcohol and was probly heavy on caustic. I'll titrate from now on.

I'm doing a weigh/heat/weigh right now and at 170* on the hot plate for 30 minutes there were no tiny bubbles nor a change in weight.
So far, so good.
I also ran a pint thru a paint funnel/strainer of Purolite and got a very clear shake up test.- 3 or 4 passes for residence time.
I dont think I would just filter and run it. I'm leery of mist washing after my new investment in resin.

Im going to North Carolina on the 3rd for a long weekend.
As I said, the bubbler just went off and soaps are not settled yet, my retention sample was used for testing. It's still cloudy but I can see all the way thru the wash tank.

?- What should I do from here? Im not pressed for fuel and have time.
This has been nearly effortless so far and would like to trickle it thru the Purolite to keep it that way.
I dont have my drywash towers completely fabbed and can use the bag filter pod with no lag tower.
Would you? and How long will this take to drop all/most of the soaps?

Thank you and I hope this helps someone else----Great Info Forum.

Brian

Corresponding pictures.

The settling bio. 3 days from reaction.


Can you see the bottom? No heat was used.


Purolite and wash test.

quote:

Originally posted by Weldshop:


I had the pretreated oil run on Cognis QTA and it came out .4% FFA and .03% moisture. 'Awesome!', I thought.
I didnt titrate. I wish I knew how to recipe from these percentages--any help there?
I entered the data into Rick da Tech's on-line calculator as T-2 KOH, 20% MeOH.



Brian

These are conversions as posted by Neutral.

FFA% = 0.766 x t for titration with 1g NaOH per litre where t is the volume of solution in ml for 1ml oil
FFA% = 0.546 x t for titration with 1g KOH per litre
neutral doesn't indicate but I would assume it's based on 100% pure catalyst.
Here is the link to the thread
http://biodiesel.infopop.cc/ev...5159#846105159

As far as the batch in the bubble jug, I would just let it sit as long as you can then run it through your magic beads or pump wash it.

Hey Brian,
Are you trying to eliminate the water wash? I always use KOH and after my troubles with straight drywashing I have a new system I am using and it works great..

If you mist wash right away you wont get that shampoo you were saying esp if the BD is hot.. Thats just a small emulsion layer that seems to be normal but I have never had a thick 1st wash.. The bubblers creat a bigger emulsion than the mist does in my opinion.

I have also filled my sock filter full of woddchips and filled the wash tank through that with good results for less washing..

Now I mist wash, dry and polish with Thermax and do it all in less than 2 days with excellent results..

I dont think I would use anything but KOH.. just my opinion..

If you have a metering pump just trickle it at 4 GPH through the Purolite and it will polish nicely.

Double D,
I will certainly read the link and study this method. I could only skim it just now. sounds very helpful.
Thank you

And yes, Lisa,
If PD206 works as directed, and the final tests pass, I could develop an S.O.P. of my own.
This oil source is as predictable as yours.
I am also studying about reflux column and condenser recovery.
I'll then also go with what works most painlessly.

I'm completely open to trying new things and methods. I suppose if I had multiple grades of waste oils, I would need to know multiple methods. 'Could happen, ya know.
And every process type I've tried so far has furthered my knowledge and experience in this hobby.
You have been much help as well.
----------------------------------------------------

Here's an observation;
I pulled some of that soap layer from the bottom drain.
I put it in a jar next to a jar of it's glycerin.
The glycerin is Coca Cola color and the soap is like a ruby red in color.

In the sample , the soap was very pale yellow. Odd.
I'm attributing this color to further glycerin dropping or amber bio in the soap.
Ive seen ruby red glycerin with sodium methylate.
It's probly a half inch thick so far in the center of the bottom/top of the poly drum.

KOH has been very easy to work with so far. Batch 3 on the K.
---------------------------------------------------------

I'll be back on the 8th of July. The reaction will be 11 days old. I'm leaving the low amp fan on until I leave.

Thanks for the replies, very encouraging.
Brian

Sounds interesting.. I'll watch your progress..
I just wont do the entire drywash thing right now after my troubles with my truck.. If I had time to let it settle days on end and all that I would but just easier to water wash a bit and move on for me.. plus the results are great so I'm gonna stick with it..
However I do sooo wish I could just process and drywash... life would be so much easier..

My 1/2 layer in the wash tank is always yellow.. I just thought this was the soapy emulsion layer..
Now when my truck got screwed up because of the soap fallout after demeth it was ruby red.. my guess is your bubbling is demething it and so you are getting the KOH soap fallout.. my glycerin is also a dark amber..
sound like you have all 3..

Have a good vacation and your goodies will be there when you get back..
Lisa

Hey,
Ya, Im sure it's methanol free or close to it. In another week it ought to be.

The beauty is that if the resin fails to reach spec, I am equipped to mist wash it after.

But. I also read that resin can raise your acid number. Who wants that? Everything else can be
on spec and the acid fall short. Would combining wash methods do this? hmm.

Let's find out!

Brian

Thats what I do.. combine them.. I guess combine them.. Wash/dry then resin dry wash.
You saw my last numbers.. the acid was okay.

May sure you settle long enough. Once your demethed if all that ruby red soap has not dropped out it will waste your resin in 1 batch... did mine and it took 10 gallons of meth to clean it.
My method now with misting 1st should make my resin last a really long time!

This commercial producer near me (I took the photos) uses ONLY wood chips to purify his biodiesel. Now as soons as I can stop procrastinating I will set up a chip tank in front of my resin lead/lag tanks as a sort of prefilter to extend resin life. I haven't used a drop of water for a year now, except a little recylcled stuff for the methanol recovery condenser.

The biodiesel still has to be demethed, which makes it easier to extract any suspended glycerine. The stuff you get on the bottom of the tank after demething is just that, suspended glycerine that has fallen out of solution.

HTH

Yeah I think we have learned that lesson. Problem is it seemed to take days to settle it all out and I dont have room or time for more settle tanks.. I also thought the resin would get any leftover soap and in my case it did not.. but it did make my resin useless in 1 batch..
The problem I have been having with the woodchips it seems great on the first pass, but the next batch I run through it will actually put the last batches soap back in just a bit. If I water wash after the woodchips, the wash water is almost a lime green..
very weird..

My pvc tower didnt stand up to the BD so if I can build another tower I may try again but for now..
I like the way I am doing it..

Thats a great setup they have going on!

Hi Legal,
I remember when you posted that about RolfQuo. I was following the whole woodchip discussion.
My problem is finding a reliable source of cheap hardwoods. I looked around. And am still open to it
if I find some.

The first thing I was told about making bio is 'Time, Temperature, and Gravity'.
The second thing was 'Water is not your friend'.

If I can stop misting all together, I will. I never did the 5% prewash.

Thanks for the reply!

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

Lisa,
I guess I dont use as much fuel as some folks. I'm pretty far ahead now. That's why I can experiment with other things.
This is just my first season making full batches. When I find what I'm going to be comfortable with and all my equipment is built, probly by next summer, I will have a routine.
I'm enjoying the learning so far.

Time and space-
Time, I have. Space, well, that's another, sad story.
I'm still in town with a small garage. I can keep things like chemicals and feedstock at work.
If I had everything I've gathered for bio at home, I would surely get some kind of citation.

I want the soap titration kit, I only need the Bromo Blue, so long as the HCL can have balm inhibiter in it.

Thanks for checking up on me.

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

This morning I ran the QTA on the bio.
Here are the results.

TG .07% Good
Acid .2% Good
Cloud 0*Celsius Good
FG .024% ASTM is .2
H2O .069% ASTM is .05
MeOH .08 Good .20 is passing

I have demethed in a few days using only a bubbler at ambient temp.
Yield is 100%.

A quick edit to my first post; it's 132 liters, not 32. More like 34 gallons.
I'm still using the little processor. The one in construction will put out 55 gallon batches.
Cant mist wash 55 gallons in this type of settling tank, but I can settle it.

I'll need to make up another so I can do 110 gallons in a weekend, transfer to a tote and begin polishing @ 5gph~.
How dose that sound?

Thanks for the support, guys.
Now I need to read up what Double D has helped me with.

Brian

quote:

Originally posted by biogirlz:
Thats what I do.. combine them.. I guess combine them.. Wash/dry then resin dry wash.

Hi Biogirl, is there any reason why you don't do a 5% prewash instead of a mist wash before drying then sending thru the resin?

I did a 5% prewash yesterday to experiment with the quality as Im moving over to dry wash.. After settling for 2 hours after the 5% pre, I had 0.7% water, and 1200ppm soaps.

Seems 5% prewash is still not effective way to reduce soaps to 500ppm the reccomended amount before shooting thru the resin beds. Wonder if mist would do a better job...

thats exactly why.. It doesnt get enough out. PLus I dont like having a little bit of wet oil left in the processor. I just decided after building the continuous drain and I didnt have to babaysit that it was easier than prewash. PLus the lady I give the glycerin to appreciates it..

Also, before you can send it to the drywash after prewash you would have to dry and demeth which we all know I learned the hard way causes slow soap fallout and longer settling times. By mist washing I get all the methanol out that way and the soaps are washed out at the same time.. My resin should last forever this way.. my fuel is actaully ready after drying but I polish it anyways just to make it that much better..

I have gotten some great fuel results with this method so I am just gonna stick with it for now even though I really wanted to get away from water washing.. catch 22!

quote:

Originally posted by biogirlz:
I have gotten some great fuel results with this method so I am just gonna stick with it for now even though I really wanted to get away from water washing.. catch 22!

Definitely!

I think if ya wanted to do strictly dry wash your methanol recovery system has to be top notch with vac set up and all the rest, to get the meth content low enough for soaps to fall out in reasonable time. Letting settle for days on end just doesn't seem practical for most who go thru a fair bit of fuel..

I agree... my buddy is still using just the drywash but I dont want to mess with the goo in the bottom of the drytank, processor and settle tanks on top of the settling time.. uuggh

I'll be home tomorow night.
I'm hoping gooey is all it will be after settling so long.

I hear of folks settling several batches before cleaning it out.

I'm wondering how easy a mistwashing will be by then.
I'll do a small sample and see.

I can switch to NaOH 99%pp if I choose to keep doing it this way.
And the new processor tank is dome topped wich I can vacum
methanol out easier with.
Both should speed things up if I understand correctly.

Brian

Yeah I didnt even consider switching to NAOH just to use my drywash...
I dont want to clean that goo at all. Did it once and thats enough.. Eevn with a standpipe I dont like it down there..

Ok, I'm home now and the batch has set for 8 days.

It looks real good and clear to the bottom. Very vivid.
The 'goo' is very thin at the bottom, maybe a half gallon or less. I see ruby red (glycerin) color.

If I used the standpipe, there would still be 5 gallons of good fuel in the tank.

So... If this process works for me, I could essentially do 10 batches before needing to use the bottom drain. That's a full tote of fuel. But with one tank, it will take 10 weeks. I'd need another
or 2 more at my pace.
Question there is, Will this goo remain flow-able, or will it set up hard?

I'll re-test everything tomorrow, I've been on the road for 10 hours today.

Brian

The "goo" I had stayed flow-able.. its just gooey. I emptied my tanks and then used my sucker to suck it over the bottom.. Flushed with BD that I drained back into the wash tank and did it again..

Sounds like a good system..