Almost ready for Prime-time

[Ford_Forgotton]

Awhile back, I promised to videotape and put on the web the steps involved in making a small batch of Bio-D. Im just letting everyone know I havnt forgotton (pardon the pun on my screen-name [img]/ubbthreads/images/graemlins/wink.gif[/img] ).

I've been slowly gathering the needed items to put on a full show and I have almost all of them.

HERE IS A PIC of what I have collected so far.

I still need a few more items to have everything, then I can setup the camera and do a little demo, encode it to windows media player, and put it on my website.

Items still to come include a Tap Water Filter by aquarium pharmaceuticals for making Deionized water for washing the pH pen in, a bottle of 99% isopropyl alchohol for making the titration mix with, and finally a jug to mix it all in!

So hopefully in the next month I can round everything up and do a nice 1000mL batch and have it come out perfect the first time.

I'll do a virgin oil mix first, then do a heavily used oil version second to show the difference in titrations. Should be fun.

All the glassware came from MacNan Biologicals (They sell a ton on ebay), The digital pH pen and calibration fluid came from National Industrial Supply (also on ebay), and got the gram scale off ebay also, but I dont remember the seller offhand. The HEET, Lye, and Oil were all bought at the grocery store. Everything in the picture adds up to just under 200 dollars in initial costs. Obviously every batch I make, the "setup costs" drop.

Oh, almost forgot. I need a rubber chicken also! That way, if anyone ever gets suspicious, I can say its a chicken BBQ!

[94_turbo]

rubber chicken--a chicken bbq??? mmuuwahhhaaaaaaaaa!!!!!!! the svo/wvo do have ways of being creative!!!!!! am waiting to see the video-----

[teester]

Forgotton, I finally made my first batch. Actually we did two single liter batches before the night was over! There is nothing like actually doing it! I made it with my neighbor chemist in his lab using his magnetic mixers. We used a mix of coconut oil and bacon grease.

We tried to titrate using Tillys Chopstick method but used a mixer instead of chopsticks. His formula called for adding drops of the .1% solution to the alcohol/oil/phenol red mixture until it first began to change color??? Then microwave it until it first started to bubble. Then while mixing, begin adding 1ml increments of .1% naoh until it turned dark purple. We put less than 1ml of the naoh in it and it turned purple! One question I have is that he said to start with a base number of 5 and add titration amount to that??? I just feel there has to be another tried and true method as we did it twice and were not too convinced of the results.

Since it turned purple immediately with the <1ml of .1%, we just used 5g naoh/liter. We used his magnetic mixer and maintained 120-135F throughout the process and mixed for 1 hour. The results were a clear separation into two distinct layers noticable in 5min.

We poured off some into a separatory funnel before settling occured and did notice what could best be described as a few globules floating on the glycerol layer after a few minutes of settling. I suspect we were a little low on the lye.

Questions.

1. Does maintaining heat in closed system allow for quicker reaction time?

2. Does heat facillitate faster separation times?

3. Big question! After doing two 1 liter batches, we only have about 6oz of glycerol. Does that sound right coming from 2400ml of total mixture? Isn't that about 10%?

Also, we heated the seperatory funnel to keep the glycerol liquid. As we did, we noticed bubbles (boiling) originating in the glyc. Is that the methanol boiling off and should we boil it all off?

We want to do a 5gal batch tonight so that we feel that we have actually been productive but I would really like to use another method to do the titration.

[rockhead55]

[ QUOTE ]
1. Does maintaining heat in closed system allow for quicker reaction time?
2. Does heat facillitate faster separation times?


[/ QUOTE ]
The reaction proceeds quicker and is driven towards equilibrium by heat (within limits of course). Seperation will also occur faster when the rection is driven towards the products we desire.

6oz seems very light ! 2.4 litres =~ 77oz I thought most people got near 20% glycerol on thorough reaction (going by memory). Were you short on methanol or lye perhaps?

You do want the methanol out of your finished bio but be very careful about boiling it off. The vapours are explosive and toxic.

Perhaps a better titration method could be looked up at the journeytoforever site.

Good luck, Glenn

[teester]

Thanks Kyoto. We washed the roughly 2 liter 50/50 with water shaking it vigorously and it didn't emulsify. I thought that if your reaction wasn't pretty much complete, you would get a lot of emulsion which wouldn't separate quickly. This stuff began to separate quickly and was back to 50/50 pretty quick with very white water! Washed it two more times and the last water was very clear. The bio also is very clear but yellow.

The oil was mostly from my Fry Daddy and was pretty clear to begin with but I don't know how you can tell how much FFA it contained.

We went ahead with the larger batch, 12L from a chinese rest. which was very dark, but smelled good! [img]/ubbthreads/images/graemlins/smile.gif[/img] We use 20% methanol in our methoxide, 2400ml this batch. About 1/4 of the lye didn't mix with the methanol and a big clump fell into the oil while pouring the methoxide in.

Upon washing a sample and waiting 5 hours, it had major emulsification (oil was still milky), a clear layer on top (methanol?), and about 1/3 white water on bottom.

I want to reprocess it as I have a new 6.0 and everyone knows, they don't need any more problems than they already have!

Any tips for how to reprocess this mess?

[jdkline]

1st reaction sounds like really high quality biodiesel. 2nd sounds like you have an incomplete reaction with a lot of unreacted or partly reacted WVO and or water and methanol in it.

[teester]

One small detail left out. The 1/4 of the lye which didn't mix with the methanol and fell into the oil NEVER DID MIX! We cranked the reactor mixer up and left it mixing at 125F for 1.5 hours, 30 min longer than the first two batches, in hopes of the lye mixing and completing the reaction. It didn't happen!

Next time I will know to drain the oil and filter off the lye and remix it with a little more methanol then try again.

Lye won't dissolve once it hits the oil!