Biopowered - vegetable oil and biodiesel forum
Biodiesel => Chemistry and process => Topic started by: greasemonkey on December 12, 2013, 03:03:40 PM
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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.
(http://i1088.photobucket.com/albums/i323/greasemonkey3/PC120022_zpse39770ea.jpg)[/URL (http://s1088.photobucket.com/user/greasemonkey3/media/PC120022_zpse39770ea.jpg.html)
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Whites and grotty oil needs really high temperatures (circa 90oC+) 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.
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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.
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You don't want to leave it too long where it is, the snow will make it even wetter !
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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 ?
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Drop it round my place. You can line it up next to Womble's soap ready for reprocessing.
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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.
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It does just look like an unreacted mixture to be fair.
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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.
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I'll try a 10/90 and see what happens.
I'll leave it till the morning now.
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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 60oC, 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.
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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 60oC, 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.
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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%.
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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.
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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.
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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.
I'd worked out for a 100L batch, using a base of 3.5, then making up 80% of that. Should I have just gone with the total figure, and not reduced it?
Should have done my homework a bit better. I do something a couple of times, think I know what I'm doing, then it comes and bites me.
Many thanks guys. I'll have it back in the reactor soon. Gonna filter down all my liquid first though. I need it for a trip, and will be caught out if it goes pear shaped again.
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Update on this.
I have added 140ml of meth/ASM mix to 1 litre of this gloop, in 20ml doses. Good black glyc dropout, but not getting any clearer.
Something went wrong with the radiator heating the reactor, and I couldn't get it over 50C. Basically, it ran low on water, I think.
So I didn't proceed any further.
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I wouldn't worry if the bio's not clear at the moment, provided you've got glycerin dropping out you have a reaction.
Try a 3/27 to find out how much of a reaction. Give the bio a good human centrifuge before testing.
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Yeah, I'll test it then and see what it says. It's still thick gloop, but towards the end I think I could see a thin film of bio settling out on the top.
If I can get the heating setup functioning, properly again, I think I'll try a palm batch, being as things are getting warmer.
I'm just wondering how much of an investment to make into the gloop now. I haven't got a huge amount of methanol to risk another 15 litres of so into another failed attempt. Hopefully, come the BBB, I'll pick up some more, which isn't so far away.
I'll persevere with the sample any how, and see what happens.
Cheers.
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Oh, you didn't say the bio was still gloopy!
The normal progression from oil is to turn thick and soapy, then go clear and very runny (can be very clear) but not drop glycerin, then go cloudy whilst staying runny and starting to drop glycerin.
You are doing these tests at circa 65°C, aren't you?
Despite it dropping or appearing to drop glycerin, try adding more methoxide and see it you can get it to the runny stage.
Of you are short of ingredients, half fill a jam jar with your gloop and grossly overdose it with methoxide ... it should prove the batch is recoverable. Then you can slowly dose the main batch bit by bit until it converts.
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This is odd stuff, it never seems to go clear, I've had it over 65, and it's still gloopy.
The batch in the reactor dropped another load of very thin glyc, and the stuff on top was thicker than the glyc, despite not having put in any chems.
I'll severely overdose, as you suggest.