Biopowered - vegetable oil and biodiesel forum
Biodiesel => Chemistry and process => Topic started by: Julian on May 19, 2013, 10:49:31 PM
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It's worked for three batches now and can only be a tribute to the way I usually manage to cock things up.
I've been two staging for many years. Since acquiring ASM, I've tried the non titration method a couple of times with reasonable success.
Three batches ago I must have been away with the fairies because I mixed ASM and methanol using 3.5 as the base amount and did an 80% stage. Realising a little later that I should have put the whole lot in and then done a 3/27, I thought blow it, (or words to that effect) and just carried on doing a two stage process. A 3/27 test after the first batch looked promising, so I drained the first stage glycerol and ran the 20% balance at the end of which I got a good 3/27 pass.
Thinking this was a little jammy I ran the next batch the same way, but with reduced catalyst. I ran the same process but used a base of 3 and got the same result. Today's batch I used a base of 2.75 and still got a great 3/27 pass. None of this accounts for any titration values ... next batch I'll do a titration.
This is the 3/27 after the first stage today ...
(http://www.palmergroup.co.uk/Bio/CBA 1.JPG)
And this after the second stage (both stages were processed for and hour) ...
(http://www.palmergroup.co.uk/Bio/CBA 2.JPG)
What's the least amount of ASM people have used to date?
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Would it be right in assuming CBA stands for "Can't be Arsed"?
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Spot testicle on!
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Nice to see you've finally posted this method (we spoke about it when I was fly tipping a small amount of soap at Julian's place).
How are those bungs holding up to bio/meths ? They look OK in the photos.
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How are those bungs holding up to bio/meths ? They look OK in the photos.
Just fine but this was the first time I've used them! They fit both my small measuring cylinders too.
The puzzling thing about this method is the reduction of ASM. I'll keep reducing it until I don't get a 3/27 pass.
Next time I think I'll try a base of 2.25g which should give me 900 ml for 80 ltrs of oil. I'm still using 15% methanol PLUS what's in the ASM, so not scrimping on that, but it's recoverable. Got about 7 ltrs out of this batch.
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I've been using a base of( 3 x oil ) x 5 for a while. The last batch I used 3 on 1st stage, then 2 on 2nd stage and still passed 3/27.
Bearing in mind everyone's oil will be of differing quality (and some people dry their oil more than others) I don't suppose this will work for everyone, There are so many variables.
Dawson
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Do you mean + oil or x oil?
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Do you mean + oil or x oil?
Yes, x oil. Typo!!
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Do you mean + oil or x oil?
Yes, x oil. Typo!!
OK, no probs, but you are doing a "complete" single stage and then a second stage to account for unreacted oil (all be it a reduced qty as per the no titration method)
I'm using 80% of one stage and then the 20% balance as per the old two stage process and therefore must be using less catalyst. I still recon further reductions could be possible.
Said it before ... the more bio I make the more I don't understand.
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I had a go at this CBA method today with somewhat disappointing results. Following the steps laid out by Julian at the start of this thread I got a 30% under-reaction from the first step and a 15% under-reaction from the addition of the balance from stage one. The disappointing aspect for me was the time taken to get to this stage. It took another 2 stages to get somewhere near a reaction I was happy with.
I ended up using pretty much what I normally do with regard to the amount of ASM used.
It was an interesting experiment that I'm unlikely to try again.
Glad it works for you though Julian.
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Sorry it didn't work for you, Nige!
I'm still playing with it though. Toady's batch was interesting ...
I tried a base of 2.5 and it would appear that that's not quite enough (when using very clean, well settled and dried oil titrating at 2, Na OH). The batch reached a yellow ochre, jelly stage after the introduction of the first stage and went no further. Upholds my thoughts that soap/gel can be caused by too little catalyst. I added 25 ml ASM ... no change, 30 ml ... no change and then 50ml at which point the colour of the batch changed to dark brown and the viscosity reduced considerably. As with the last batch there was a two degree temperature rise which held stable for nearly an hour in a very in a poorly lagged processor.
Samples taken shortly after the temperature rise were most unusual, very nearly completely clear, but with no glycerine drop out when human centrifuged. A 3/27 test gave a massive drop out of about 50%.
Two further additions of 50ml sent the samples cloudy, they quite readily dropped glycerine and gave only a small drop out in a 3/27 test.
There's still the second stage to run for this batch, but I think I've reached the limit of ASM reduction. Next batch I'll go back to a base of between 2.75 and 3.
Don't know what use all of the above is but the very marked difference betwen the gel and clear phase was fascinating in a sad anorak type of way!
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Forgot to post the pic I took of the mid batch clear sample. Bear in mind this is straight out of the processor during the first stage ...
(http://www.palmergroup.co.uk/Bio/mid_batch_sample.JPG)
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Completed this batch today by only using ½ the remaining ASM/methanol from the second stage. That makes a tad over 1000 ml for 80 ltrs of oil.
If you take the figures on the wiki page as gospel you come out with a figure of 2800 ml. Dawson is obviously using far less catalyst and I know many others are. I think we should revise the wiki page so the base of 5 is replaced by 3.5 or even 3 if the titration value is accounted for.
Do others agree? Jim, do you have any comments as I think they were your figures in the first place?
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Do others agree? Jim, do you have any comments as I think they were your figures in the first place?
I wasn't aware I ever advocated a base of 5, I started with 4 and now down to 3.
The 5 is the multiplier use to adjust g/ltr NaOH to ml ASM.
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Completed this batch today by only using ½ the remaining ASM/methanol from the second stage. That makes a tad over 1000 ml for 80 ltrs of oil.
Julian, where on earth did you get the 2800ml of ASM from? If I were doing an 80ltr batch stage one would be 15% methoxide, including the methylate, using a base of 3 giving 960ml of ASM.
No wonder you've made so much soap in the past.
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((5.0 + 2.0) X 150) X 5 = 5250mL of methylate
is what's on the wiki page, 5 being both the base and multiplier.
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http://www.biopowered.co.uk/wiki/Processing_with_anhydrous_sodium_methylate
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2800 ml was achieved by the following ... (base 5 + titrated value of 2) x batch of 80 x multiplier of 5
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2800 ml was achieved by the following ... (base 5 + titrated value of 2) x batch of 80 x multiplier of 5
I think the confusion is between single stage and two stage amounts.
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2800 ml was achieved by the following ... (base 5 + titrated value of 2) x batch of 80 x multiplier of 5
I think the confusion is between single stage and two stage amounts.
Forgive him for he knows not what he's doing.
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No confusion on my part!
I haven't been doing no titration processes, I've been doing an 80/20 two stage split of a single stage. The formula for which, off the wiki page, is above.
The difference being I've been ignoring the titration value and reducing the base which seems to have reached a minimum of around 2.75 - 3.
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No confusion on my part!
I haven't been doing no titration processes, I've been doing an 80/20 two stage split of a single stage. The formula for which, off the wiki page, is above.
The difference being I've been ignoring the titration value and reducing the base which seems to have reached a minimum of around 2.75 - 3.
Never believe everything you read.
As ASM doesn't generate water a reduction of 1 - 1.5g/ltr on the base Number would be a good starting point BUT as we all have different oil suppliers, mixes of veg and plants we have to find the best base for our individual setups.
3 works for me atm with the veg I'm getting.
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Julian--
I think I know why with the reduced ASM you had a fully clear and no drop-out result.
There wasnt enough Glyc derived, therefore the small amount that was, was insufficient to make the meth/glyc dense enough to settle. The Bio/di/mono glycerides also present formed a Co-Solvent with the meth resulting in the clear fluid you made....
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Julian--
I think I know why with the reduced ASM you had a fully clear and no drop-out result.
There wasnt enough Glyc derived, therefore the small amount that was, was insufficient to make the meth/glyc dense enough to settle. The Bio/di/mono glycerides also present formed a Co-Solvent with the meth resulting in the clear fluid you made....
Whoosh ... about 50% of that went straight over my head! Will it translate to Noddy speak?
I'm just running another batch now and I've created the same effect, but this time I've taken samples at three stages ... I'll post a photo later, see if it gives you any more of a clue.
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I'd be using 1800ml ASM made up to 22.5ltr for S1. and expect 80ish% conversion.
What are you using?
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I'm following this thread closely, I reduced my ASM to a grand total of 2.98 base for the last batch.
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I tried taking a photo but due to a dramatic reduction in Global Warming in the Surrey area, there wasn't enough natural back light to prevent the flash going off. For that reason the photo's not too good and the two right-hand samples look the same.
I'll have another try tomorrow in the hope that Global Warming will be back up to the levels that dictate everyone has to pay more tax.
Here's today's photo anyway ...
(http://www.palmergroup.co.uk/Bio/Three stages of conversion.JPG)
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I'd be using 1800ml ASM made up to 22.5ltr for S1. and expect 80ish% conversion.
What are you using?
I'm following this thread closely, I reduced my ASM to a grand total of 2.98 base for the last batch.
I'm still rather playing at the moment. I've lately been working around a base of 3 and ignoring any titration values, so for my 80 ltr batches 1200ml, but on the last couple of batches I've had to add additional ASM, probably because the oil may be quite a high titration. I didn't measure the additional ASM, just used little "glugs".
Anyhow on both the last two batches a base of 3 has been too low, but I've used it as a starting point and then been guided by the various phases, colours, clarities and temperatures as to how much more ASM to add.
On today's batch I got the highest temperature rise yet, 4°C and by studying carefully I had a static temperature on the second stage for in excess of half an hour ... this on a very poorly insulted processor.
On the last two batches I've assumed that the end in the rise in temperature on the 1st stage was the reaction going as far as it would go and settled the glycerine as soon as the temperature started dropping.
Similarly today with the second stage I assumed all the time the temperature was static, the reaction was taking place. When the temperature started to drop I did a 3/27 which gave a reasonable pass. That made the reaction time for the second stage about 20 minutes.
20-30 minutes is about the duration of the 1st stage temperature rise.
Still lots of things with which to play.
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There you go. Global warming is doing it's bit for photography. Managed to get a shot of 4 samples against what little light we seem to get in a British summer these days ...
(http://www.palmergroup.co.uk/Bio/Three stages plus water wash.JPG)
Now the samples have been sitting over night the gel has gelled a bit more and glycerine has settled.
Left to right ...
1) Under dosed ... Gel, very thick forms skin on hot sample and drips solidify. Almost solid after 24hrs.
2) Add a little catalyst ... batch changes colour, clarity and viscosity to biodiesel consistency, exothermic reaction is noticeable by a couple of degree temp rise. No glycerine drop.
3) Add still further catalyst ... batch stays thin but goes cloudy and will drop glycerine.
4) After 2nd stage with 1st stage glycerine added back, demethed and 7% water washed.
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So let me get this right (to make sure I've followed this correctly),
if we react wet/damp oil a good amount of the catalyst gets eaten up forming soap,
this can produce something like sample No1. (I know you've underdosed on catalyst but the same will apply),
Adding more catalyst will bring the reaction forward to your No2 and No3 samples,
then it's just a case of a normal second stage.
This is what I have done recently and had good results (in the reaction, not so good when washing).
So that big drum of soap that some kind person dellivered to you should be esay enough to turn into sparkling bio.
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I should say this thread has rather drifted, but it's all to do with reducing ASM quantities. First off I had several batches where I could get a complete reaction using bases of around 3.5-4, whilst ignoring the titration value. I suspect on those batches, the oil would have titrated low if I'd bothered to check.
In emulating that process on other oil I've come across these "phases" of conversion. Realising that jelly seemed to be a function of too little catalyst, I just carried on adding and ended up with a good conversion.
So yes, you've pretty much got it, except the oil was as dry as I could get it. Dried with a condenser at over 100°C ... I haven't yet tried it with knowingly wet oil. Could be worth a jam jar size batch to try.
If you remember when you were round fly tipping your soap, I'd done some experiments with soap and glycerine. That produced a substance that didn't give a 3/27 result at all, but was clear and liquid and would process normally into bio. I recon I'd hit the second phase in the photos above using the catalyst remaining in the glycerine ... all same glycerine washing.
I've done some jam jar tests on your soap and grossly over dosing with catalist pushed it to reasonable bio. So I'll shortly bite the bullet and try a whole batch slowly dosing until I get the phase changes and temperature rise.
Are you going to ask for it back now? Don't forget you'll have to convert it with the next couple of weeks.
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Oh, I should have said that in getting the first stage to drop glycerine, I used about half of the 2nd stage catalyst, so the second stage wasn't really a normal 20% but more like 10%.
One other thing I've been trying is throttling the pumps when processing. Having seen the vid of the guys with the gear pump, I've tried throttling the combined output of the Leo and the Mono to 50 psi whilst still having a small flow. Don't really know if this has made a difference, but the second stage converted in 20 mins. I guess I should really try one thing at a time!
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Oh, I should have said that in getting the first stage to drop glycerine, I used about half of the 2nd stage catalyst, so the second stage wasn't really a normal 20% but more like 10%.
One other thing I've been trying is throttling the pumps when processing. Having seen the vid of the guys with the gear pump, I've tried throttling the combined output of the Leo and the Mono to 50 psi whilst still having a small flow. Don't really know if this has made a difference, but the second stage converted in 20 mins. I guess I should really try one thing at a time!
If you had a decent 'ductor you wouldn't need to throttle back output to increase the inpump mixing.
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I was trying to create cavitation after the valve!
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Are you going to ask for it back now? Don't forget you'll have to convert it with the next couple of weeks.
No I'm not asking for it back, I'd rather the batch was saved and the method reported on.
I just don't have the time to mess about with it now.
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I've just completed another batch using remarkably low ASM levels.
Total consumption of ASM was equal to a base of 2.88 with 16.5% methanol
!00ltr batch, 1440ml ASM and 16.5ltr of methanol
A 180lt batch would equate to 2592ml ASM and 29.7ml methanol of which I would expect to recover 9lt from the bio only.
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Are you seeing the "gel" stage at all?
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Are you seeing the "gel" stage at all?
I don't see any stage 'cause it all happens in the reactor, once I've put the WVO in to the Drying tank I see nothing 'til the bio comes out into me cubie ready to fill the jam jar.
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Well, get a proper jam jar and take frequent samples during processing ... you may be surprised.
PS I've given Mike your email address, so he should contact you soon if he hasn't already done so.
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Well, get a proper jam jar and take frequent samples during processing ... you may be surprised.
PS I've given Mike your email address, so he should contact you soon if he hasn't already done so.
I take my sample in a good quality Whisky Tumbler, nothing as common as a jam jar.
Been talking to Mike via email all afternoon, could be making the trip Saturday.
I've bet him I can bore him to death before he to gets me, reckon I'll win.
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Really nice, interesting chap ... I mean Mike, not you!
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Really nice, interesting chap ... I mean Mike, not you!
Thanks MATE.
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Hey, we learnt everything from you Jim, you should be proud!
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I've just completed another batch using remarkably low ASM levels.
Total consumption of ASM was equal to a base of 2.88 with 16.5% methanol
!00ltr batch, 1440ml ASM and 16.5ltr of methanol
A 180lt batch would equate to 2592ml ASM and 29.7ml methanol of which I would expect to recover 9lt from the bio only.
How much of the 16.5% used was reclaimed and was it used in stage 1
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How much of the 16.5% used was reclaimed and was it used in stage 1
I measure out the ASM add ALL the reclaimed from last brew then top up with virgin, approx 9% on this batch.
BTW stage one produced an 84% conversion.
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I don't seem to be able to get as low as Jim, but then I've had some pretty grotty oil of late. I use all my reclaimed methanol from the previous batch which works out to be about 30% of the methanol for the new batch.
I'm currently using a sort of suck it and see method using the "phases" that seem to occur which are detailed earlier in this thread. I use a low dose to start circa base of 3 or a little more and ignore the titration. This usually generates a "gel". I then add small amounts of ASM in a little methanol (I have tried neat ASM in bio but it can solidify) until the "phases" change and the process temperature rises. Processing for about ½hr after that or until the process temperature drops, which ever is the longer, appears to give a very nearly complete reaction. Second stage need only be about ½ the normal amount for a second stage to get a good 3/27 pass.
After a 7% water wash soap levels seem to be very low as, last batch, I only need 20ml of sulfuric to neutralise 80 ltrs of bio.
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I don't seem to be able to get as low as Jim, but then I've had some pretty grotty oil of late. I use all my reclaimed methanol from the previous batch which works out to be about 30% of the methanol for the new batch.
I forgot to mention that the methoxide on stage one was injected via the venturi at 80+C due to an oversight on my part (forgot the heater was on).
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He, he. I've done that while waiting for glycerin to settle ... took me ages to work out what was going on!
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With low soap levels you should be able to drop the acid wash completely,
give it a go, you can always add some acid if it doesn't work for you.
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With low soap levels you should be able to drop the acid wash completely,
give it a go, you can always add some acid if it doesn't work for you.
Hmm, that's a thought butadding acid is a good insurance policy!
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With low soap levels you should be able to drop the acid wash completely,
give it a go, you can always add some acid if it doesn't work for you.
Hmm, that's a thought butadding acid is a good insurance policy!
Insurance yes,
but my last couple of batches using ASM only needed two or three washes,
and I was using more catalyst than you.
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With low soap levels you should be able to drop the acid wash completely,
give it a go, you can always add some acid if it doesn't work for you.
Hmm, that's a thought butadding acid is a good insurance policy!
Insurance yes,
but my last couple of batches using ASM only needed two or three washes,
and I was using more catalyst than you.
Depending on what you count as a wash, that's pretty much all I'm doing ... 7% water wash with all the glycerin (while I'm not making logs, and acid wash and one straight water). Batch I did yesterday only required 12ml, but I'd still rather stick the acid in than run the risk of an emulsion.
BTW ... Had a bash at melting your soap with a tosser tube today (after I'd spent ½hr cleaning all the gunge off the lid if the barrel). It only took a little heat from a tosser tube and a bit of stirring to get it to a point where the Mono will pump half the barrel into the processor.
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BTW ... Had a bash at melting your soap with a tosser tube today (after I'd spent ½hr cleaning all the gunge off the lid if the barrel). It only took a little heat from a tosser tube and a bit of stirring to get it to a point where the Mono will pump half the barrel into the processor.
Lets hope it doesn't set sold in the pipes.