Biopowered - vegetable oil and biodiesel forum
Biodiesel => Chemistry and process => Topic started by: thewormman on June 04, 2013, 05:07:01 PM
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Posted this on VOD to...
Just doing first batch and inevitably got distracted and screwed up now dont know where to go from here.
OK 180 litre batch, 2 stage no tit using ASM. All chemicals brand new.
Dried oil all ok. Up to temp in processor, distracted by something else got quantities wrong :(
So was meant to be for the first stage: (3.75 base)
Methanol volume = 12% X 180litres = 21.6 litres,
methylate volume = 5 X (3.75 X 180) = 3375ml
ACTUALLY put in
Methanol volume = 24.6 litres,
methylate volume = 375ml
I know call me a dick...
So when I noticed tried to add missing ASM and process. Noticed oil coming back out of venturi think It may have blocked... soap???
It is in the processor still at about 60C So this is where I am and I dont know what to do from here HELP
Pic of what is in there now
(http://i250.photobucket.com/albums/gg244/zukenstein/Bio/first/Photo7_zps27377c32.jpg) (http://s250.photobucket.com/user/zukenstein/media/Bio/first/Photo7_zps27377c32.jpg.html)
Put some in a jar with some more ASM
(http://i250.photobucket.com/albums/gg244/zukenstein/Bio/first/Photo8_zps4062367f.jpg) (http://s250.photobucket.com/user/zukenstein/media/Bio/first/Photo8_zps4062367f.jpg.html)
Another jar with some meth added
(http://i250.photobucket.com/albums/gg244/zukenstein/Bio/first/Photo9_zpse4049b1a.jpg) (http://s250.photobucket.com/user/zukenstein/media/Bio/first/Photo9_zpse4049b1a.jpg.html)
Did a 10/90
(http://i250.photobucket.com/albums/gg244/zukenstein/Bio/first/Photo6_zps45377053.jpg) (http://s250.photobucket.com/user/zukenstein/media/Bio/first/Photo6_zps45377053.jpg.html)
About 8ml drop out I guess most of it hasnt converted but with all that meth what do I add?
Let the torrent of derision begin, and please then tell me what to do!!!
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Well we all end up making mistakes, as is human nature - but you've put an artificial burden on yourself by starting with a high complexity - so I'll berate you for not just doing a single stage, small batch for your first batch and working forward from there.
So what I'd expect from a two stage:
Methanol: 180 * 0.2 * 0.8 = 28.8 litres. I think you've got enough in for first stage anyway.
Methylate: 180 * 3.75 * 5 * 0.8 = 2700 ml.
In both calculations, the 0.8 at the end is so you only put in 80% of required, as per two stage process.
You seem to have calculated 80% Methanol but the full amount of Anhydrous?
In any case, nothing you've done so far should result in the venturi failing to work, so I'm wondering how you dried your source oil?
I take it you don't have enough Anhydrous in there to make up 2700ml because of the lack of suction?
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Calculations I used came from Jamesrl
I only put 375ml of ASM in at first then tried to add the rest later when I realised, but when I tried it just stopped going in now the venturi doesnt suck at all. :(
Really I just need an experienced eye to tell me based on what I have what to add next. The ASM I put in the jar sample has turned to jelly BTW :(
I can suck anything needed in before the pump as I put a sight tube in so can use that, just dont want to make it worse or a disaster.
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Also Oil was dried through diffuser in separate tank at 65C with hot air also blowing on it. Three and a half hours, did a hot pan test got no reaction and continued to dry for another 20 mins
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Well the only way you get jelly is if water is present.
Your Methanol, are you sure that's virgin and not reclaimed?
Do you have a spirit hydrometer to test it?
Certainly adding the quantity of Methanol you have, and the limited amount of ASM, should definitely not have caused jelling. You have water present somewhere.
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Well the only way you get jelly is if water is present.
Your Methanol, are you sure that's virgin and not reclaimed?
Do you have a spirit hydrometer to test it?
Certainly adding the quantity of Methanol you have, and the limited amount of ASM, should definitely not have caused jelling. You have water present somewhere.
Meth is virgin from Trinity dont have a hydrometer :(
Introducing that much ASM with very little meth in it when I was trying to correct my mistake would that have caused a jelly reaction as it met the flow of oil in the pipe?
Thanks for taking the time to answer :'(
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I've played quite a bit recently with jelly/soap and had success by continuing to add methanol and ASM.
It looks like you've tried adding both separately to samples. Try a large overdose of both ... say half a jam jar of gel from the processor mix about 50ml methanol and 5ml ASM and add that, put a lid on and shake like crazy. Sit in a bath of just boiled water and see what happens.
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These are the results of doing exactly that ...
(http://i41.tinypic.com/a25fgl.jpg)
The soap is solid and the bio very nearly clear.
Not important for your current problem but I've got a gut feeling that many reactions go through a gel/soap stage during the addition of the catalyst. If that's the case, by underdosing you may have reached that point without proceeding to a full conversion.
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Great! Got so involved is posting that I just missed bidding on a Mono ... I was going to try a speculative bid of £15 ... it went for £13.55, bugger!
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Wow sorry
The answers are appreciated :)
Have just tried dosing in a jar with both it is settling now
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Great! Got so involved is posting that I just missed bidding on a Mono ... I was going to try a speculative bid of £15 ... it went for £13.55, bugger!
Use gixen, it doesn't forget!
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Great! Got so involved is posting that I just missed bidding on a Mono ... I was going to try a speculative bid of £15 ... it went for £13.55, bugger!
Use gixen, it doesn't forget!
I remembered I wanted to bid and the end time. I had a dedicated window open. Checked that there was 5 mins left and thought I had time to put up the post and get back to the auction, swapped back the window having posted just to see 1 and then 0 seconds come up in the timer!
Posting took far longer than I thought.
I quite enjoy bidding live, I can get within about 3 seconds, but as senility sets in I guess I ought to give gixen a try.
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I've played quite a bit recently with jelly/soap and had success by continuing to add methanol and ASM.
It looks like you've tried adding both separately to samples. Try a large overdose of both ... say half a jam jar of gel from the processor mix about 50ml methanol and 5ml ASM and add that, put a lid on and shake like crazy. Sit in a bath of just boiled water and see what happens.
I am really busy at the moment and tried to squeeze doing my first batch into a short day and really I think I rushed at it to much.
I left it hot overnight and have drained the oil down today into cubies. I am going to take the pipe work off and check to see if I blocked something by adding all that ASM with virtually no meth. As was said the only way the venturi could be leaking oil is if there was some back pressure. The main valve was open at the top and there was only 200 litres in there with the meth so I need to take the pipes off and have a look.
There was not really any glyc so nothing had reacted really. No soap no jelly oil looked same as when it went in really.
On the su99estion of Julian I did a mini batch in a jar with the oil that came out, scaled it all down and it seems to have reacted ok, although the 10/90 i did on it the colour of the meth looks a bit strange. Have attached a couple of pics what do you think?
(http://i250.photobucket.com/albums/gg244/zukenstein/Bio/first/Photo5_zps21c1cda5.jpg)
(http://i250.photobucket.com/albums/gg244/zukenstein/Bio/first/Photo4_zpsb82de874.jpg)
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The top picture shows you have a good amount of gly dropped out, nothing wrong here.
The meths in the second picture looks fine, it'll get tanted with the colour of the bio.
And you only have a very small amount of dropout, so with this in mind reduce the amount of catalyst when you do the rest of the batch,
this will then leave a reasonable amount for the second stage.
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Cool thanks Mark my panic is subsiding :)
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You say no soap, no jelly ... so just oil?
Soooo, no reaction until you add more catalyst and methanol.
If you can recall what you added, I'd just sling the balance in and see what happens.
To follow on from the jam jar test, had you have had jelly, if that converts just add methanol and catalyst until you notice a change from a thick sort of yellow ochre to a dark brown, less viscous liquid.
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Processed everything ok this time. Thanks for the help :)
I have washed the bio and when I tested with one of Nigels soap testing kits it came out as 16.7 PPM so well pleased.
Before I start to dry I just want to confirm everything is OK to proceed because the final wash water came out like this.
(http://i250.photobucket.com/albums/gg244/zukenstein/Bio/first/lastwash_zpse2c28a2a.jpg) (http://s250.photobucket.com/user/zukenstein/media/Bio/first/lastwash_zpse2c28a2a.jpg.html)
Should I continue washing till its clear even though the soap tests low?
Thanks
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You may find that water will clear if you leave it for a while.
How sure are you of the titrated soap test result? It's often difficult to discern the colour change especially when the soap count is low.
I think you're pump washing in the processor aren't you ... if so I'd run at least on additional wash, just to compare water samples. It's so little hassle with this method and it's always best to err on the safe side.
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Ok perhaps I'll do a hot wash and test it again as that one was at ambient. I did the soap test on the previous wash as well and it was at 30.4PPM so seems to be in the right direction and what I expected. Thanks for the input