Biopowered - vegetable oil and biodiesel forum
Biodiesel => Chemistry and process => Topic started by: Jamesrl on February 02, 2013, 07:24:53 PM
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Wish me luck, I'm about to put 10ltr of hot-ish water with 17.5ml of 98% sulphuric acid into 100ltr of perfectly reacted bio.
I do hope it don't go belly up.
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Jim you will be fine (trust me I'm a doctor)
Hopefully you will find like others that its so much easer this way
Paul
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Good luck Jim. Hopefully not with your new cottage industry Mayo :)
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Good luck, let us know the result
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Your post reads like you were going to add the water to the acid! In which case all the wishes of good luck will be most useful.
I'm sure you know, but for others reading, you should always add the acid to the water and slowly.
It really is a good method, I'm sure you will get good results.
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Jamesrl, water washing !!!
Has hell frozen over ?
Are we sure this is the same jamesrl ?
Do we have an imposter amongst us ?
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He's not posted in the last two hours.... hopefully that 98% acid hasn't dissolved his trumpet (or anything else come to that)
I used the last of my concentrated Sulphuric acid up last week. I am now onto the 20+ litres of 85% Phosphoric Acid that I have tucked away.
Whilst I'm sure it could still do some damage, it seems a whole lot less scary than the Sulphuric did.
I must remember to make up a new titration fluid with the Phosphoric though otherwise things could go rather wrong
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Hi Julian
Do you want some dry acid when you come up next week.
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I'm not sure that there would be a lot of point as I would have to add it to the water anyway to get it in to the batch.
Worth a go if you are donating samples though.
It looks like all systems are go for Friday, should be up just after lunch if that is OK and will have a trailer full for you.
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It does mix with water much safer than 98% sulphuric and @ 5g pL it brings the ph down to 1 so should be easy to make up a good and strong 25L tub at a time then just add required amount to the batch rather than having to mix acid with water to get the acid in the batch.
Yes I have a bag of samples going out for trials
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did a batch myself a couple of days ago, after doing a quick 5% water wash with the left over glyc in there i did my normal 40ml of acid and 10litres of water, no problems, have now done another 3 x 10litres pump washes and all is well,
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Yes it' is me doing water washing with acid and feck it's cold here, cold enough to freeze hell.
Julian, I did add the acid to the water, I might be mad but I ain't daft.
What I did.
I mixed 1ml of sulphuric to 1lt of deionised water as atitration solution.
Ipa and 10ml of Bio (after a good 10/90 with zero dropout) on me Mag stirrer with the blue stuff in it
I used 1.75ml to neutralize the caustic so 1.75/1000ths of concentrated acid to 10ml of Bio.
0.00175ml = 10ml,
0.175ml = 1ltr,
17.5ml = 100ltr
So 17.5ml to 10ltr of water for the first wash.
Not only did I use the pumps but engaged all three Eductors to boot, NO mayo, whopeee doppee do.
Second wash coming up.
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Cool
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Cool
No, it's hot.
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What made you try this jim, is it just out of curiosity or necessity?
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At this rate it'll be "Drywash corner" at the BBB with just three blokes in it :o
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What made you try this jim, is it just out of curiosity or necessity?
Disbelief ! ! !
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What made you try this jim, is it just out of curiosity or necessity?
With so many going on about it I had to give it a try.
It's more time consuming, hand on wise but hopefully a quicker finished product.
It was the low volume of water that swung it for me.
I'll give it a few batches before I decide which way to continue.
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Give the acetone wash a try, uses even less water and is quicker.
http://www.biopowered.co.uk/wiki/Using_acetone_to_aid_soap_removal
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I do the acetone stage now.
I do the acid wash first then stop, wait for a couple of hours and drain it.
Then, for 300 litres of bio, I add 45litres of cold water with 100ml of acetone mixed into to it. It really does seem to pull out the contaminants quicker.
Two batches in a row have given a clear 50/50 shake test after just the acid wash and one acetone enriched water wash.
Not sure of the soap ppm as I need some more chemicals from Nige (which I will collect next weekend).
I am tempted to try acetone in the acid wash so what happens.
I cant see that anything nasty is likely to form. I know that Acetone and Hydrogen Peroxide in the presence of Sulphuric acid can form TATP which is explosive but then that needs concentrated chemicals and becomes explosive when dry. As there is no Hydrogen Peroxide anywhere near the process and it is only small quantities of chemicals mixed into loads of water and bio, I can't see any real problem.
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Jim
Pretty pleasing to see you giving it a go. U gonna try the acetone next time too?
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All done, it took four 15ltr washed to get a good 50/50. I gotta get me some Acetone for the next go.
Now riddle me this, I took a sample from the last wash, let it settle and split took some of the Bio and did a 50/50, nice clear water phase.
I drained down the 15lt from the reactor and it's like milk.
??????????????
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All done, it took four 15ltr washed to get a good 50/50. I gotta get me some Acetone for the next go.
Now riddle me this, I took a sample from the last wash, let it settle and split took some of the Bio and did a 50/50, nice clear water phase.
I drained down the 15lt from the reactor and it's like milk.
??????????????
I'm so happy reading this I almost have a tear in my eye. :'(
It doesn't follow that if you have 'unclear' wash water then the 50/50 or soap tests are going to be poor. And remember that the crap is in the settled water and not in the bio.
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What made you try this jim, is it just out of curiosity or necessity?
With so many going on about it I had to give it a try.
It's more time consuming, hand on wise but hopefully a quicker finished product.
It was the low volume of water that swung it for me.
I'll give it a few batches before I decide which way to continue.
No reason you cant do both is there?, washing if you need fuel in a hurry or for winter and settling at other times maybe
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All done, it took four 15ltr washed to get a good 50/50. I gotta get me some Acetone for the next go.
Now riddle me this, I took a sample from the last wash, let it settle and split took some of the Bio and did a 50/50, nice clear water phase.
I drained down the 15lt from the reactor and it's like milk.
??????????????
Got a theory about this... well here goes!
I wonder if the meth reduces with each wash rather than in just one wash, with the subsequent washes the meth ppms or % reduces. When it gets to a critical low level it suddenly releases the greatest concentration of soaps.
If this is true it would explain how you can get fairly clear discharge water on one wash and then the water on the next wash seems more cloudy. I've seen this on the odd occasion with gradual mist washing, can't recall seeing it with pump washing though, so not sure how or if it's likely to be true with pump washing. It's only a theory, no other evidence to suggest that it's true.
If I was making bio at the mo, I'd use my shiny new meth tester (compliments of KH) to add some numbers to the idea.
I'll sit back now and await the ridicule :-))
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No ridicule at all. That is a very plausible explanation.
I guess it would be worth doing soap testing on the fuel after each wash and recording the PPM
If there is a sudden drop between, say, the third and fourth wash then that would support your theory.
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I would think that the soap will reduce inline with the reduction in Methanol, as it is fully water soluble, and will come out as easily as the meths when washing. I can't see the soap sticking with ever reducing amounts of methanol until a 'critical' point where soap is released - I can understand that when demeth and settling but not when water washing.
I would be interesting to see results of meth vs soap after each wash though.
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Sadly, until I get a new processor, I'll have to stand on the sidelines. But the tests mentioned should be easy enough to replicated and demonstrate or dismiss.
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I'm doing a batch tomorrow,
this is going to be split in two for a comparison test, standard pump washing V acetone washing.
To get comprehensive results I'll be doing titrated soap tests at every stage of the washing,
these results may help with your theory.
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I forgot to mention the fact that the bio had been demethed within an inch of it's life before it was Acid washed.
As no one seems to have mentioned their drying methods I went into condenser drying with the Squirrel merrily working away. At 85°C there was a small but steady flow of water, after 90mins of demething and a few litres in the cubie I transferred the bio to the settling tank and turned on the bubbler. The last time I checked it it had changed from orange juice to a nice dark bio looking liquid.
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The last time I checked it it had changed from orange juice to a nice dark bio looking liquid.
Are you saying that it was orange juice when it went into the settling drum after 90 mins drying?
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The last time I checked it it had changed from orange juice to a nice dark bio looking liquid.
Are you saying that it was orange juice when it went into the settling drum after 90 mins drying?
It was still a little wet, not as orange juicey as a 5% prewash, just been out to check it it's really clear now.
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The last time I checked it it had changed from orange juice to a nice dark bio looking liquid.
Are you saying that it was orange juice when it went into the settling drum after 90 mins drying?
Jim is your Bio dark due to feedstock or demething at high temperatures and bubbling.. ie: oxidised maybe
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Jim is your Bio dark due to feedstock or demething at high temperatures and bubbling.. ie: oxidised maybe
Neither it's the storage tank, I took a sample and it light and crystal clear.
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The last time I checked it it had changed from orange juice to a nice dark bio looking liquid.
Are you saying that it was orange juice when it went into the settling drum after 90 mins drying?
It was still a little wet, not as orange juicey as a 5% prewash, just been out to check it it's really clear now.
I'm surprised. The last two batches which haven't turned to soap, have come out of the processor really clear, looks like it could go straight in the car. I didn't pay much attention to how long it took, but I'd guess an hour under heat to around 85°C and probably another hour without heat down to about 50°C ish using only the venturi and condenser (compressors and aquarium pumps are banned until further notice), add Coldflow, pump out and no bubbling in the settling tank!
For how long did you settle the last wash? I did 5 washes to get clear water. On the last two washes, samples cleared from orange juice to cloudy in around a couple of hours.
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The last time I checked it it had changed from orange juice to a nice dark bio looking liquid.
Are you saying that it was orange juice when it went into the settling drum after 90 mins drying?
It was still a little wet, not as orange juicey as a 5% prewash, just been out to check it it's really clear now.
I'm surprised. The last two batches which haven't turned to soap, have come out of the processor really clear, looks like it could go straight in the car. I didn't pay much attention to how long it took, but I'd guess an hour under heat to around 85°C and probably another hour without heat down to about 50°C ish using only the venturi and condenser (compressors and aquarium pumps are banned until further notice), add Coldflow, pump out and no bubbling in the settling tank!
For how long did you settle the last wash? I did 5 washes to get clear water. On the last two washes, samples cleared from orange juice to cloudy in around a couple of hours.
How are you drying the air going into your venturi Julian ?
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The last time I checked it it had changed from orange juice to a nice dark bio looking liquid.
Are you saying that it was orange juice when it went into the settling drum after 90 mins drying?
It was still a little wet, not as orange juicey as a 5% prewash, just been out to check it it's really clear now.
I'm surprised. The last two batches which haven't turned to soap, have come out of the processor really clear, looks like it could go straight in the car. I didn't pay much attention to how long it took, but I'd guess an hour under heat to around 85°C and probably another hour without heat down to about 50°C ish using only the venturi and condenser (compressors and aquarium pumps are banned until further notice), add Coldflow, pump out and no bubbling in the settling tank!
For how long did you settle the last wash? I did 5 washes to get clear water. On the last two washes, samples cleared from orange juice to cloudy in around a couple of hours.
How are you drying the air going into your venturi Julian ?
It's just circulated through the SHHE and condenser as per normal GL operation.
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Whats a SHHE
" https://www.google.co.uk/search?q=SHHE&oq=SHHE&aqs=chrome.0.57&sourceid=chrome&ie=UTF-8 "
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What does Google know? Try the wiki ...
http://www.biopowered.co.uk/wiki/Acronyms
and ...
http://www.biopowered.co.uk/wiki/Still_head_heat_exchanger
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What does Google know? Try the wiki ...
http://www.biopowered.co.uk/wiki/Acronyms
and ...
http://www.biopowered.co.uk/wiki/Still_head_heat_exchanger
Oh I have one of them. 8)
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Got a theory about this... well here goes!
I wonder if the meth reduces with each wash rather than in just one wash, with the subsequent washes the meth ppms or % reduces. When it gets to a critical low level it suddenly releases the greatest concentration of soaps.
If this is true it would explain how you can get fairly clear discharge water on one wash and then the water on the next wash seems more cloudy. I've seen this on the odd occasion with gradual mist washing, can't recall seeing it with pump washing though, so not sure how or if it's likely to be true with pump washing. It's only a theory, no other evidence to suggest that it's true.
I don't think you're too far from the truth there Nathan. No great shakes on your theory...that's how I've seen it since day one. The amount of methanol and soap in solution are directly related to each other when water washing. As the volume of methanol in solution gets less the more soap drops out until the eurika moment where the bio goes from an orange juice appearance to something that looks like proper bio. As I've said on many occacsions I can reach this point in approx 4 x 10lt washes without the need of adding chemicals in an attempt to speed things up.
I'll do some testing on this on my next batch...I'll soap test after each wash.
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Got a theory about this... well here goes!
I wonder if the meth reduces with each wash rather than in just one wash, with the subsequent washes the meth ppms or % reduces. When it gets to a critical low level it suddenly releases the greatest concentration of soaps.
If this is true it would explain how you can get fairly clear discharge water on one wash and then the water on the next wash seems more cloudy. I've seen this on the odd occasion with gradual mist washing, can't recall seeing it with pump washing though, so not sure how or if it's likely to be true with pump washing. It's only a theory, no other evidence to suggest that it's true.
I don't think you're too far from the truth there Nathan. No great shakes on your theory...that's how I've seen it since day one. The amount of methanol and soap in solution are directly related to each other when water washing. As the volume of methanol in solution gets less the more soap drops out until the eurika moment where the bio goes from an orange juice appearance to something that looks like proper bio. As I've said on many occacsions I can reach this point in approx 4 x 10lt washes without the need of adding chemicals in an attempt to speed things up.
I'll do some testing on this on my next batch...I'll soap test after each wash.
Thanks Nige
B nice to see some data around this on soap... can this be correlated to meth % with meth tester?
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So if this is correct, and I suspect it is, demething the bio before washing could reduce the amount of washes needed.
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I'm absolutely sure that a meth test on consequtive washes will show an incremental reduction everytime.
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Got a theory about this... well here goes!
I wonder if the meth reduces with each wash rather than in just one wash, with the subsequent washes the meth ppms or % reduces. When it gets to a critical low level it suddenly releases the greatest concentration of soaps.
If this is true it would explain how you can get fairly clear discharge water on one wash and then the water on the next wash seems more cloudy. I've seen this on the odd occasion with gradual mist washing, can't recall seeing it with pump washing though, so not sure how or if it's likely to be true with pump washing. It's only a theory, no other evidence to suggest that it's true.
I don't think you're too far from the truth there Nathan. No great shakes on your theory...that's how I've seen it since day one. The amount of methanol and soap in solution are directly related to each other when water washing. As the volume of methanol in solution gets less the more soap drops out until the eurika moment where the bio goes from an orange juice appearance to something that looks like proper bio. As I've said on many occacsions I can reach this point in approx 4 x 10lt washes without the need of adding chemicals in an attempt to speed things up.
I'll do some testing on this on my next batch...I'll soap test after each wash.
Thanks Nige
B nice to see some data around this on soap... can this be correlated to meth % with meth tester?
It wont mean to much without it.
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So if this is correct, and I suspect it is, demething the bio before washing could reduce the amount of washes needed.
How much methanol would you expect from the bio alone? Would the time and effort put in be outweighed by the volume recovered. Bare in mind the reduced methanol now being used in two stage no tit methods.... would it be worthwhile?
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I'm absolutely sure that a meth test on consequtive washes will show an incremental reduction everytime.
That would make sense, but it would be good to see if the soaps drop in a fairly linea way, if not is there a meth % that sees an increase in the amount of soaps released? It would be an elegant answer to what can be seen from time to time, ie 50/50 clear on one wash, with the next wash producing a more cloudy 50/50. It's not too important as going through HW shavings seems to do the job, but it's nice to be able to explain observations.
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Demething does reduce water washing, but with new ways of pump washing with 2 or 3 buckets of water, is it worthwhile?
Steve, tried this I think prior to water washing?? I can't remember what he said about it.
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So if this is correct, and I suspect it is, demething the bio before washing could reduce the amount of washes needed.
How much methanol would you expect from the bio alone? Would the time and effort put in be outweighed by the volume recovered. Bare in mind the reduced the methanol now being used in two stage no tit methods would it be worthwhile?
It may not be worthwhile when doing non tit (I'm down to 16% meths now), but for others that are still titrating there may be some gains.
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Agreed
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Jim
What are your conclusions about water washing?
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Demething does reduce water washing, but with new ways of pump washing with 2 or 3 buckets of water, is it worthwhile?
Steve, tried this I think prior to water washing?? I can't remember what he said about it.
The reason I was going to demeth before washing was simply because I was experiencing methanol fumes with every wash and even when the wash water was clear I got meth fumes when drying !
The next batch I made was with Acetone and it settled so quickly to a clear 50/50 I found it was not worth washing.
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It may not be worthwhile when doing non tit (I'm down to 16% meths now), but for others that are still titrating there may be some gains.
I'm only using 10 - 11% virgin + ASM + reclaimed.
And yes I think demething IS worth the time and effort, less than 30p to get 4-5ltr of methanol back.
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James
Now you're potentially on board with us strange water washing types. What can you do to shorten drying times in a sealed system (simplest possible method) to at least as comparable with a spray bar ring?
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James
Now you're potentially on board with us strange water washing types. What can you do to shorten drying times in a sealed system (simplest possible method) to at least as comparable with a spray bar ring?
I partially dried the wet bio using the condenser AND squirrel and finished off in the settling tank with the Bubbler.
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James
Now you're potentially on board with us strange water washing types. What can you do to shorten drying times in a sealed system (simplest possible method) to at least as comparable with a spray bar ring?
I partially dried the wet bio using the condenser AND squirrel and finished off in the settling tank with the Bubbler.
Nothing new then.
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James
Now you're potentially on board with us strange water washing types. What can you do to shorten drying times in a sealed system (simplest possible method) to at least as comparable with a spray bar ring?
I partially dried the wet bio using the condenser AND squirrel and finished off in the settling tank with the Bubbler.
How long did this take? The spray bar / ring thing dries in less than an hour. In a sealed system it'd be good to have something comparable!
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James
Now you're potentially on board with us strange water washing types. What can you do to shorten drying times in a sealed system (simplest possible method) to at least as comparable with a spray bar ring?
I partially dried the wet bio using the condenser AND squirrel and finished off in the settling tank with the Bubbler.
How long did this take? The spray bar / ring thing dries in less than an hour. In a sealed system it'd be good to have something comparable!
Exactly the same system as most demeth with will work for drying mate.
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i would just like to add i just read all this thread, i got nothing to offer, but all the same a very interesting read !
ok im done :)
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James
Now you're potentially on board with us strange water washing types. What can you do to shorten drying times in a sealed system (simplest possible method) to at least as comparable with a spray bar ring?
I partially dried the wet bio using the condenser AND squirrel and finished off in the settling tank with the Bubbler.
How long did this take? The spray bar / ring thing dries in less than an hour. In a sealed system it'd be good to have something comparable!
Exactly the same system as most demeth with will work for drying mate.
Cool! On the new system then!