Emulsion, or not converted?

[greasemonkey]

100 litres of real bad oil. Glyc wash, leave circulate for 1 hour, at around 55c. About 10 litres of glyc in. After settling for an hour, drain about 40 litres of muck out the reactor, consistent in quantity with the sample I took.
Add back a further 30 litres of good WVO, so back to 100 litres.

1400ml of ASM, 12 litres of methanol. Circulate for one hour, at above 60c.

This is what I have. No separation, no dropout.

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[Julian]

Whites and grotty oil needs really high temperatures (circa 90^oC+) to make it usable.  I don't glycerine wash but I'd have treated the bad oil first to get it to a reasonable state added the good oil and then glycerine washed.  If you have any doubts about the oil always do a HPT.

Try taking a sample and whack in a bit more methanol and ASM.  You'll get a reduced yield, but you should get some yield.

[greasemonkey]

I wasn't really expecting to get that amount of gunk out of the  bad oil after glyc washing. Now, I've pulled about 150 litres out of the reactor into drums, so I don't know what the heck is going on.
I'll do some experiments with it, see what happens.
For some reason, it's now going solid.

[1958steveflying]

You don't want to leave it too long where it is, the snow will make it even wetter !

[1958steveflying]

I wasn't really expecting to get that amount of gunk out of the  bad oil after glyc washing. Now, I've pulled about 150 litres out of the reactor into drums, so I don't know what the heck is going on.
I'll do some experiments with it, see what happens.
For some reason, it's now going solid.

On a serious note you had a reaction with a total of 112 litres and yet you have now drained 150 litres out, am I missing something ?

[Julian]

Drop it round my place.  You can line it up next to Womble's soap ready for reprocessing.

[greasemonkey]

I wasn't really expecting to get that amount of gunk out of the  bad oil after glyc washing. Now, I've pulled about 150 litres out of the reactor into drums, so I don't know what the heck is going on.
I'll do some experiments with it, see what happens.
For some reason, it's now going solid.

On a serious note you had a reaction with a total of 112 litres and yet you have now drained 150 litres out, am I missing something ?

I think it's me who's missing something. I'm slowly coming coming to the conclusion that I had far more oil in there than I thought I did. I did my workings for 100 litres, so have one third less chemicals than I needed. That would explain a lot.

It must be unreacted. There was a perfect split after the glyc wash, and i know the oil I added after was hardly used. I hardly think it's an emulsion, the last time I tried this I had the pipe work full of water, and that came out OK.

[1958steveflying]

It does just look like an unreacted mixture to be fair.

[julianf]

Try 90/10 and see if it all drops out.

Id have got it hotter too.  I know youre using ASM, but, at this time of year, i run everything on the hot side, as it means that there's less chance of things getting blocked on the settling.

[greasemonkey]

I'll try a 10/90 and see what happens.
I'll leave it till the morning now.

[Julian]

I'll try a 10/90 and see what happens.
I'll leave it till the morning now.

Why you no rissen!

The answer to every problem (apart from world peace and why Jim's been banned from the VOD) is to add more catalyst and a bit more methanol.  You can see it's under reacted, I've got 200 litres of under reacted bio sitting in the garden that I've been stairing at for 6 months.

Heat the sample to around 60^oC, slowly add  premixed catalyst and methanol whilst string (beware fumes) and watch it change to a lovely clear golden liquid.  But it doesn't end there, no Sir, because as nice as it looks it won't drop any glycerine at this stage ... add a bit more methoxide until it starts to go translucent.  Give it a damn good stir and then leave ... you'll be pleased with the result ... honest.

[greasemonkey]

I'll try a 10/90 and see what happens.
I'll leave it till the morning now.

Why you no rissen!

The answer to every problem (apart from world peace and why Jim's been banned from the VOD) is to add more catalyst and a bit more methanol.  You can see it's under reacted, I've got 200 litres of under reacted bio sitting in the garden that I've been stairing at for 6 months.

Heat the sample to around 60^oC, slowly add  premixed catalyst and methanol whilst string (beware fumes) and watch it change to a lovely clear golden liquid.  But it doesn't end there, no Sir, because as nice as it looks it won't drop any glycerine at this stage ... add a bit more methoxide until it starts to go translucent.  Give it a damn good stir and then leave ... you'll be pleased with the result ... honest.

In will, don't worry. I'm not so concerned about an emulsion now.

[Glycer-rides]

GM, am I correct in thinking your glyc wash was with just 10% glyc?

If so, that's way too low. it won't remove all the water.
For crappy oil, I'd be looking at using 30%.

[Jamesrl]

GM, you'd under dosed the ASM and methanol even for a 100ltr batch

You should be looking at 1500ml ASM with 13.5ltr meth, never start with less than 15% of the batch volume of methoxide.

Your sample looks like a lack of chemicals.

[greasemonkey]

GM, am I correct in thinking your glyc wash was with just 10% glyc?

If so, that's way too low. it won't remove all the water.
For crappy oil, I'd be looking at using 30%.

Yes, around 10%. Maybe I ought to leave the worst stuff alone till I build up a bit more glyc.