Latest report from Mickey

17% batch passes Warnqvest.
Mickey just Teletyped me that he has just Checked his latest 50 litre batch and it passed the Warnqvest test.
It was immediatly clear and bright and no drop out.
This batch was made from Palm oil titrating 2.5 using Neutral's new recipe as stated above using 140ml methanol in the first stage and 30ml methanol in the second stage.
Process time for each stages was 1.5 hours with a holf hour wait for the glycerine to settle.
Reaction temperature was in excess of 50deg C

I would like to report the results of a batch that I am working on.
75 liter of WVO, titrate at 4.1
Decided to use 18% methonal and the two stage process that has been discussed here. As mentioned above by Chris, I used 4.29 grams base plus 4.72 (titration of 4.1 x 1.15) for first stage and 11.35 liters(total for the first stage) of methanol. Added this to 130 F. oil over 30 minutes and mixed for 70 minutes and let settle for 2 hours. Drained the glycerine and used .8 grams NAOH per liter of oil in2.27 liters (total for the second stage)of methanol. Mixed for 1 hour and left it to settle over night as it was getting late. This morning, it was 48 F. in the shed so I tried to heat up a little methanol and bio from the batch to about 60 F. and tried the 27/3 test and there was NO drop out, however it was a bit cloudy. I took it inside the house and when I got home this evening the beaker was clear and still no drop out.
I noticed that there is a thick layer (soap??) on top of the bio in the reactor that I have not tried to skim off yet. Otherwise, it looks like my other batches at this stage. I will start washing in the AM.
Thanks for the info in this thread.

16% test batch passes Warnqvest

Latest report from Mickey
Flush with his recent success, Mickey has just made a 16% Methanol mini- batch that passed Warnqvest.

Mickey used Neutral's New recommendation for KOH/NaOH amounts with a modification in Methanol amounts.
Oil was Palm titrating at 2.5
Each stage was reacted for 1.5 hours.
Passed Warnqvest- Immediatly clear and bright with no drop out.

Stage 1 4.9g KOH+ (Titration X 1.2)mixed into 137ml methanol.
Stage 2 2.1g KOH mixed into 23ml methanol

Tilly or Neutral. I am very interested in testing this new base/base method. I am currently using the GL One-Day process with great results but recognize that the savings in methanol costs alone would be worth investigating this process.
I am using NaOH and routinely titrate at 2.75-3.0gm/l. I am getting a little lost and confused jumping around trying to find a good 'recipe' with which to begin. Can you point me in the right direction?

Hello fatkid

I suggestthat you start with a few mini-batches and see how things work out

I tried a method similar to this on a large batch in an appleseed and it failed the 3/27 test.
Here is what I did.
The batch was 95 liters and titrated 2.5g KOH. I multiplied this by 1.2 and used a base of 8.7. This meant that I used 1112 grams of KOH.
I used 90% of the KOH in 13.3 liters of methanol. This was 1000g in 13.3 liters of methanol. I reacted this in my appleseed with a static mixer for 2 hours at 140 F. I then settled the glycerin for ~20 minutes and drained. I then mixed 112G of KOH in 2.2 liters of methanol. I mixed this with the oil for 2 hours in the appleseed.
It failed the 3/27 test with a large amount of dropout.
What do you think I did wrong?
I don't think it was my equipment as I have made about 100 batches with this setup.
I was wondering about bumping up the methanol a little bit. The reason that I tried this was to conserve methanol, so I would love to get it to work with as little methanol as possible.
Thanks,
DD

Hello Dandy don

I recommend that you do a few mini-batches using Neutral's formula exactly and see what happens

Tilly

A word on agitation. I suspect that KOH may work better than NaOH in the 2-stage reaction because the product glycerine is more liquid so agitates more easily. There could be a clue here as to why some bulk batches do not go as well as in glassware. In glass you can start with a few seconds hard shake. Nothing beats that for agitation. In bulk the agitation may be a lot less and in the 2-stage economy process you have minimal methanol in the first stage and the viscosity will higher than normal and may impede agitation sufficiently to slow down the reaction. If this happens longer stirring will not help as the side reaction will have destroyed the catalyst. Could explain a few observations.

DandyDon

Is there any possibility of you loosing methanol due to evaporation? With methanol numbers this low, you have to be REALLY sure that you are not loosing methanol. If you have VERY fine calibrated temperature control, then 140F might be ok. Otherwise, back down the temperature a little. Maybe 135F ? Make sure your chemistry works in 1 liter test batches before scaling up, then make sure you are not loosing methanol. Are you open-vented during processing? Do you have a recovery coil on the vent?

Overall quantities of KOH are pretty much the same, but this is probably a lot less methanol than you have been using. Not much room for error or loss on the methanol quantities.

Chris

I am going to try this on a large batch with NaOH instead of KOH. I will let you know how it works out.

Thanks for your helpful suggestions!
No I don't think it is due to methanol loss. I do have a condenser on the vent so any methanol that does go up the vent condenses and runs back in.
I don't think it is due to agitation as I do have a static mixer and added the methanol very slowly.
I just did a single stage batch with the same amount of KOH and 20% methanol reacted for 3 hours that passed the 3/27.
As far as doing small batches and then scaling up. I have always had problems getting things to work on the bench top and then starting all over again when I scale up as the equipment and dynamics of the reaction are different. I will do a few small batches, but will still need your help in trouble shooting whatever goes wrong.
DD

Okay, I did a big batch this way.
Here’s my try at Neutral’s base/base with a large batch and NaOH.
Parameters: Soy WVO titrating at 2.67. Use base of 4, so 6.67 grams/liter. 25.23 grams/gal. 100 gallon batch, pump mixed with gerotor type pump at 36 gpm. Elbow/nozzle in tank just below oil level to swirl-mix tank and preclude aeration of oil. Good vortex in tank when pump is running.
Add 2325 grams NaOH to 14 gallons of methanol while heating oil. Slowly add methoxide to suction side of pump (about 12 minutes). Mix for 1.5 hours after addition of methoxide. Processing temp 144 deg. F (62.2 C) Settle for 1.5 hrs. drain off glycerin. Restart pump and heater. Return to 140 degrees. Add 378 grams NaOH to 2.3 gallons methanol. Introduce slowly to suction side of pump. Mix for 1 hr. Settle (1 hr.) and drain glycerin again. Go to bed. Next morning, drain glycerin again and take some BD with it. Remove sample from top of processor and perform Warnqvist test.
Cleared up in about 4 minutes, no drop out! I am a happy camper!
Warqvist picture:

Comments?

Joe,

Sounds great! The pump you have sounds like it really gets things moving.

One question though - in the pic it looks like there is a tiny bit of darker yellow oily stuff at the bottom. That is not a trace of precipitate, is it?

Andrew

Hello Joe

I am relieved.
I was worried for a while. I thought this may have been one of those chemical reaction that only works in the Southern hemisphere.
I am glad you performed the reaction with NaOH.

So do you think we could safely conclude that whether you are reacting 1 litre, 50 litres or 378.54 litres the chemistry does not change and should work equally well in any part of the world for the average homebrewer?

Andrew,
The picture's not that great, but it's clear and no precipitate at all. The bottom of that little glass jar is all dimpled.

Tilly, I even had the vortex going in the proper direction for the northern hemisphere. Didn't want to take the chance of messing it up by going against the coriolis effect. Who knows, maybe that would make a more vigorous mix.

Tilly,

quote:

So do you think we could safely conclude that whether you are reacting 1 litre, 50 litres or 378.54 litres the chemistry does not change and should work equally well in any part of the world for the average homebrewer?

Guess we need to find someone else with a 36 gpm pump to replicate? Will a static mixer with a weaker pump also replicate this?

If this can be replicated elsewhere, it supports the theory that better mixing (or quicker turnover) allows us to use less cat and or methanol. Right?

Andrew

Hello Andrew

Yes, exactly.
And also, because the sun is higher in the sky in the tropics at lunch time, This chemical reaction might not work in the tropics.
We need to get someone located in the tropics (Northern or Southnern Hemisphere would probably suffice) to do some tests.
I wonder, should we also do these tests both east and west of the prime meridian? It has been my experience that the world East of the prime meridian is VERY different from the world west of the prime meridial. Surely with such a difference, chemical reactions are likely to be different too.

I also notice that we have jumped from 50 litre batches to 378.54 litre batches.
Noone has proven that the chemistry works in in 127.36 and 251.79 litre batch.
Someone needs to get onto this too.

Yes, I think it may take several years to determine whether this procedure will work in every part of the World for every size reactor likely to be encountered in a Home brewing situation.

quote:

Originally posted by Andrew Morris:
Guess we need to find someone else with a 36 gpm pump to replicate? Will a static mixer with a weaker pump also replicate this?

Andrew

Andrew,
I have a larger pump because of the larger processor, I wouldn't expect the HF pump to do a good job on a 100 gallon batch, even with a static mixer. (don't tell Murphy I said that )Try it, though and let us know. I believe one must size the pump to the processor. True, maybe my 36 gpm pump will work on a larger processor as well, I just don't have one bigger than the 130 gallon one I've got. I have a 550 gallon one, but it has a 125 gpm pump for it. It's not completed yet. The 36 gpm pump is a gear pump, the 125 gpm pump is impeller. Next 100 gallon batch I will reduce mix time and see how it fairs. I like the methanol savings with this method, even though it takes a little longer.

Joe,

Yes your pump is bigger because your processor is bigger.

Just that your pump is bigger in a perportional sense as well as an absolute sense. My pump is about 7 gpm (HF or NT - same) and I use 32 gal. of oil. Your pump moves about 5 times as much oil and your batch is about 3 times as big.

I am not sure if all these relationships are linear, but better flow rate could be the answer.

I wonder how much of the benefit you get is the bigger pump and how much is the the mixing you get inside the tank.

Ideas or tests anyone?

Andrew

So boys, what did I do wrong?
I have thought about the whole pump volume idea. But the fact that I can get a single stage with 20% methanol to pass the 3/27 with the same oil, same equipment and same solutions confuses me a little.
I can try it with NaOH and see what happens?
Any other ideas or suggestions?
Thanks,
DD