So, lets hear all the naysayers about how you do not want to add water to your reaction.

I do 30 gallons of oil as my base due to processor size, (or lack thereof)

And I was always annoyed by the length of time it took to dissolve my catalyst. So after reading Tillys' recent thread about his experiments with this old aqueous method and favorable (IMHO) results, I gave it a shot. my catalyst was dissolved instantly, my fuel is looking good so far. I seperated 2 batches last night using this process, and they are being spray dried as I type this. I know of all the people trying to reduce methanol evaporation using GL's "no water" wash. But I bet we are releasing more methanol to the atmosphere from our processors which are vented to the outside, than we are releasing using the "dry-wash" method to remove this material so the soaps will fall out.


So, here is my process:

30 gallons WVO, titrated at 2.6 gpl, 5.0 GPL as a base, 6.6 gallons of methanol. 30.4 ounces sodium hydroxide dissolved in 1 gallon of water. and then added to my alcohol, process temperatre near 125-130 farenheit. added water/alcohol mixed over a period of 25 minutes before the pump (to take advantage of the natural pressure differentials) Processed for 1 hour 25 minutes. added 5% water to the mix, circulated for another 30 minutes, pumped it into my standpipe seperating tanks overnight. transferred into my "spray-dry" drum this afternoon, and it is drying as we speak. In an open environment of course.

My expectations are to have the soaps coagulate and fall to the bottom of the drum, so I can then transfer the fuel to a clean drum, filter the lot to remove any suspended soaps. let my buddy burn 15 galons in his truck, watch results, and then use it in my Bobcat if this process meets my normal yields within a gallon or two.

Since I never could find the correct ratio's for the conc. aqueous method, The 1 gallon water was a guess at best, and it seems to have worked. I was always bothered by the amount of heat generated in a highly flammable medium of alcohol, and was suprised at how hot the water got in this process. (wear gloves!!!, it gets hot!!!)

anyone else use this method? any questions? any comments? what was your purpose for trying this method? any failures? What are the correct ratio's for the water? anyone know? if so, please tell me.

I will post more of my results as they happen, i've Been working more than I prefer, so my replies may come later than expected.

Hello Big Makwa

The correct ratio is close enough to 1:1 by weight, NaOH to water.

30.4oz= 862g
So you should have used 862ml of water, that is slightly less than 1 US quart.
You certainly used enough water.

thanks for posting the proper ratio's Tilly,

Are you still using this method?

I was expecting much more soap formation from this method. but it seems ok.

Hello Big Makwa

If I were still making biodiesel I would still be using the Cons Aqueous method!

I think I know the answer to this question before I ask it, but I'll ask anyway.

Has anyone successfully tried this method with ethanol instead of methanol?

This also makes me wonder how important de-watering is before processing?

Steve,

You said you used to make it that way, did something occur (emlusion, glop, etc) that made you change your method?

quote:

Hello Big Makwa

If I were still making biodiesel I would still be using the Cons Aqueous method!

Tilly,
You're not making biodiesel any more? Is the Earth about to stop spinning? Have you gone SVO?

Please explain.

Oh, I get it .

"Don't ask don't tell" and other odd metaphors.

Sorry to hear that you are no longer making biodiesel, Tilly. But, I understand that to conform to the people's will is of the utmost importance. Where would civilization be without good citizens.

Very good of you to assist all of us ignorant imperialists in our quest for cheap fuel.

Long live the Empire.

I have been using 45% liquid KOH/water with success here.

Another benefit of this method would seem to be the reduced concern over small amounts of water in methanol that is recovered through methanol recovery. Any thoughts on that?

ok, I finally got a day off to finish the "two" conc. aqueous batches I started a week ago.

I obviously used way too much water!!! Way too much. Does anyone need any soap? I got some to spare!!!

so, after doing this method wrong (too much water) i still have nice clear clean fuel with about a 1.5 gallon loss to soaps. But that is most likely because of my huge water addition.

So, I am going to try & find the time to get 2 more 30 gal batches done the correct way today and report back.

I did use a 5% pre-wash,settled and I washed without water after settling & seperating near 24 hours.
I skimmed off near a full gallon of cottage cheese-lookn soap off the top after spray-dry aeration and settling, and found another half gallon on the botom.

So besides the soap amount, this process still saved me at least 1 hour of hands-on time required to properly dissolve my catalyst. Well worth it to me. since I can cut 5 acres of grass while the process is running unattended and while I am waiting for the oil to heat.
I am expecting much less soap with these forthcoming batches now that Tilly has enlightened me to the proper ratio's (thanx Tilly)
Why can't I find a recipe for this method anywhere?


so here are my plans for these next 2 batches.

30 gallons of oil, 5 grams base, plus titration of sodium hydroxide, mix in less than 1 liter of H2O, (instead of a gallon or more) then added to 6.6 gallons alcohol. process at 130 degrees F, for 1.5 hours, add 2.3 gallons hard water for prewash, pump into standpipe tank overnight and sepearte and spray dry the next day to hopefully see way less cottage cheese on top.

I cannot believe I ignored this old method for so long, I credit Tilly's revival of this method from a previous post( that he does not use because he doesn't make bio anymore) to saving me from carpal tunnel syndrome from rocking a 15 gallon HDPE drum back & forth for an hour or more. and subsequently generating heat & pressure inside this plastic drum containing a highyl flammable and toxic substance.

Hello steved

Do I understand correctly that you are talking from vast experience? Perhaps you could share with us your experiences using the Cons Aqueous NaOH method.

I have a dream that one day this nation will rise up and live out the true meaning of its creed: "We hold these truths to be self-evident: that all men are created equal." I have a dream that one day on the red hills of Georgia the sons of former slaves and the sons of former slaveowners will be able to sit down together at a table of brotherhood. I have a dream that one day even the state of Mississippi, a desert state, sweltering with the heat of injustice and oppression, will be transformed into an oasis of freedom and justice. I have a dream that my four children will one day live in a nation where they will not be judged by the color of their skin but by the content of their character. I have a dream today.

Sorry steved, nothing about koh in this dream

Hello steved

In other words you have never tried the Cons Aqueous NaOH method and have not got a clue what you are talking about.
I always find it refreshing when a person presents himself as an expert at something he knows nothing about.

quote:

Originally posted by steved:
tilly, i have been doing it long enough to know when someone is pulling my leg. about making biodiesel anyway.

Hello steved
And in my dreams this site remains a forum where people can freely discuss different ideas an production procedures without being concerned that they will be ridiculed and made fun of by someone who does not know what he is talking about.

quote:

Originally posted by steved:
yes, and in my dream, i use koh and i burn my biodiesel unwashed. i have learned not only how to master the biodiesel making but also the soap making. my filters last forever ........

Hello steved

One would assume Big Makwa was referring to Naysayers that actually knew what they were talking about.
If you had started your attacks on this method and the people using it by saying what you were writing was your dogmatic view based on having never researched the method and not having any experience or knowledge whatsoever with the method it would have cleared things up.

You are new to the forum and obviously do not understand there is a longstanding "Rule" that people can discuss most any production idea they wish to without fear of being ridiculed and made fun of by someone who does not know what they are talking about.
It is also a forum rule that when people introduce "New" ideas they also post the justifies for this information.

The Cons Aqueous NaOH method is a "Mainstream" production procedure that has been well researched and documented on this forum and is used by a large number of people.
Do a bit of searching on this forum and find out what Neutral's tests showed.
I have posted test results too as have others.
Neutral was also a fellow who did not agree with using the Cons Aqueous method. But that did not stop him from keeping an open mind and doing some tests.

Hey Tilly,
I've been hanging around here for a few years and greatly appreciate your input.

I have to admit that you used to be a lot more fun, but I don't care.

Your help has been critical.
Thanks

Hello Steved,
When you say you "love" me I hope that you mean that in the same way a person loves a classic automobile or a glass of fine scotch.

Cons is how we abbreviate the word Concentrated in ลึก ประเทศอินเดีย. It is just one of those strange features of the local dialect.
Looking back at some earlier posts I notice It used to be Conc Aqueous NaOH. English is apparently a changing language.

ok, I have settled on a final procedure.

I will continue to use the conc. aqueous method with the revised water addition figures, ( thanks again Tilly)But I also add the water to the alcohol before adding my catalyst. I found this to be a hapy medium between long dissolve rates, and the amount of heat generated by ading the catalyst to the water alone and then vaporizing the alcohol with that superheated water.
and I am using Grahams waterless wash with great success.
I also collect all the soaps generated from this process and use it as a goopy handwash to clean up before I go back into our home. I find it nice to actually see the amount of soap generated from making my fuel instead of just seeing cloudy wash water get spread across or gravel parking lot.
I have noticed about 1 gallon less yield per 30 gallons feedstock compared to my old way of production.

I do use between 5-7% water prewash with settling for 24 hours. I spray-dry and skim the cottage cheese/rice krispies off the top, and change barrels every couple hours to remove the congealed soaps off the bottom & sides. with a final filtering of 5 microns before storage in 15 gallon HDPE drums. I opened a drum after sitting about 1 month with no residue present on the bottom and no spooge or Mung present on the sides either.
The fuel was clear and without chunks.

Although there is a foul smell generated from this process that I never noticed in the past. maybe it is just my feedstock?

I have a question that relates to this thread and several in Methanol Recovery. As I understand the Conc Aqueous method, you can have an equal amount of water in the reaction up to the weight of the catalyst. If you were recovering your methanol and on one batch you recovered 5 liters that was 80% pure (1000grams water), shouldn't you be able to use that methanol "as is" in your next batch as long as you needed at least 1000g of catalyst? The reason for asking is, if you are recovering methanol, is it really necessary to build a reflux still or do multiple distillations to get the purity as close to 100% as possible?

I jsut used the liquid method. i like it!
not going back to powder. Found a place to get
liquid premix for 42 cents a lb. much easier to use.