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Author: Subject: Whole batch demething (Volunteers needed)
Chug
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[*] posted on 17-3-2009 at 01:17 PM
Whole batch demething (Volunteers needed)


I had been doing some experimenting over the w/end with 30L batches and as they were much smaller than my usual batches I decided to try something different, because I would end up losing a lot less bio than normal if things went wrong, and to be honest, after all I have read on the subject of reversing the reaction, I was expecting it to go wrong! but I have also read that some commercial companies recover from the whole batch using high temp and vacuum., so it got me thinking.

**************************************************

Experiment:

I performed my modified version of the 2 stage process and without performing the prewash
see post here
http://www.vegetableoildiesel.co.uk/forum/viewthread.php?tid=11808&page=1...

So I then tried demething the batch whole, YES the whole batch of bio and glyc, that is without draining off the glyc first, something which you can read everywhere that will allegedly reverse the reaction and unmake your bio back into oil again.

I performed a 3/27 with no fallout before the demething and I did it to what looked like good biodiesel after demething the whole batch and I still got no fallout, so it seemed like it was good bio and it had not reversed back to oil, a shake em up water test also seemed to confirm it was good bio, but maybe it was a fluke.

So I decided to repeat this whole batch demething experiment with another of my 30L modified 2 stage batches and got the same result, so now I need to try it again on my usual 135 litre batch.
If this works repeatedly then it will save time and energy not having to settle and drain glyc and on not reheating glyc back up from cold to demeth it

I would like to ask if someone else with GL style processor with venturi and condensor would try demething a small batch with the glyc stil present and see if it works ok for them.

It certainly beats messing about with acid to neutralise the catalyst which is the accepted way to demeth from the whole batch.

Just do your reaction as normal but instead of settling and draining the glyc off, just move straight from reaction to demething, once demethed settle and drain glyc within an hour or two as it will soon go solid without the methanol or prewash water present.

UPDATE: After setttling for a day or two I find that there is not any more soap than normal in the bottom of the settling tank from these batches that I didn't do a prewash on, if anything there was less soap.


EDIT: This is a long thread and my method has evolved slightly so you may just want to skip to the latest version here.
http://www.vegetableoildiesel.co.uk/forum/viewthread.php?tid=11912&page=2...



[Edited on 24-9-2009 by Chug]




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[*] posted on 17-3-2009 at 08:50 PM


How much meth did you condense off Chug?

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[*] posted on 17-3-2009 at 08:52 PM


And how pure was it.
Stop jumping about Nige, I can't keep up with you. I'm 83 and not as nimble as I used to be.




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[*] posted on 17-3-2009 at 10:31 PM


Measuring the recovered meth was one thing I didn't think of as I was scratching my head trying to cover the bases on the other new factors and keep everything the same. And I already had some recovered from a prewash batch in the drum to start with, but it should have been pretty pure as there was no prewash, but I suppose there could have been some trace water from the side reaction of ffa-soap that may have gotten in there.
But it'll get used up anyway so no worries.

Try it on a small batch and let me know how you get on.





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[*] posted on 18-3-2009 at 12:19 AM


I have a GL type reactor.
When the reaction have finished all I do is stop the pump, off with the heater and leave overnight. I Don't prewash!!!!
In the morning drain off the glis and demeth.
From an 80l mix I get aprox 2-3l of meth.
The meth is aprox 95-6% pure.
Not adding the prewash keeps the mix water free and the meth comes out very good.
Then put into the wash tank for 60l wash, then dry, then into settle tank for at least a week and any soaps left drop out.
All of my water free glis is then saved till i get aprox 60l and that goes into a separate Hot water cyclinder and I remove all the glis to 95-6% pure. If i take to much off the quality goes down to 85% so I use that for other purposes (Rayburn Mix)
The 95-6% I use in Bio production.
Saying all that I've not made any for two months as I'm in sunny OZ and will have to come home mid April so hope all are keeping warm
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[*] posted on 18-3-2009 at 10:40 AM


bioplumber, have you actually demethed the whole batch as in this thread, or are you saying you will give it a go?



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[*] posted on 18-3-2009 at 11:19 AM


Hmmm... Two radical changes in one batch..... Should I????


Mike




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[*] posted on 18-3-2009 at 11:56 AM


Yes Mike,

but maybe only try it on a small batch just in case I'm barking!




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[*] posted on 18-3-2009 at 12:11 PM


I'll run an 80 litre batch this weekend....

It would be interesting to get Graham's views on this. Anyone know what he's up to - he's not posted here since before Christmas?

Cheers

Nick
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[*] posted on 18-3-2009 at 12:55 PM


That could save me a lot of time,effort and electric, I will try with a 250 ltr batch that I will process on Sunday,the only difference is that I am useing an elux reactor and drive the Methanol out with compressed air ,should get the same result though.....
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[*] posted on 18-3-2009 at 01:02 PM


Chug, As you know I do the acid neutralisation of the caustic and then demeth the whole batch, the last batch I made I added 7% prewash before demething.

I`m going to be brewing Thurs or Fri this week and I`ll try your suggestion of just adding the stage 1 glyc back into the batch then add 7% prewash to kill the reaction then demeth the lot. :smiley-whacky097:




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[*] posted on 18-3-2009 at 02:18 PM


it was following your whole batch progress stumpy that got me reading up on this and deciding to risk it on a small batch, and I'm still suprised it worked!

I ran my whole batch method past the chemist neutral from the infopop forum, and it could be that leaving the 1st stage glyc in helps to use up the excess NaOH and he says we know the biodiesel reaction comes to a dead stop eventually if there is not enough NaOH and he says I may well be on to a good method, reducing complexity, and he is interested to hear how it turns out for others.



[Edited on 18-3-2009 by Chug]




DISCLAIMER:
Safety is your own responsibility, satisfy yourself it's safe, don't take my word for it!
1992 709D Mercedes
1983 Dodge 50
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1994 Citroen ZX 1.9 TD, Engine now in 1996 Peugeot 306
http://www.biofuel-uk.net/
http://www.biodieselcommunity.org/


GOVERNMENT WARNING!:
If you are having individual free thoughts please switch on your TV immediately and watch x factor, or go shopping, or buy a happy meal, free thought will lead to extremism. It is harmful to the collective good and won't really make you happy. The democratically elected world leaders have your best interests at heart and will do everything within their power to make sure everyone is equal and safe from terrorism and infectious diseases and recession. Please help by consuming as much as you can and following all orders without question!
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[*] posted on 18-3-2009 at 09:22 PM


If it is because the reaction comes to a stop isn't that what we achieve when we do the 5% prewash (or am I missing something ----- again!)
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[*] posted on 18-3-2009 at 10:26 PM


I'd think - when we do the prewash WE are stopping the reaction, but if it comes to a stop of it's own accord - surely this is better? As it means a more complete reaction??


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[*] posted on 19-3-2009 at 10:42 AM


CHUG!!!! I have for the last 6 Months always done my reaction in the manor described.
Reaction, then turn off, then leave overnight, then drain off glis, demeth the bio (Aprox2-3l of meth taken off at aprox 95-6%).
Then put into wash tank, use aprox 60l water, dry and put into settle tank for at least a week and then use.
Save glis and when enough distll meth of aprox 60l of glis and get aprox 35-40l meth at 95-6%.
So far no problems.
I decided not to use prewash as it introduced water to the system and that would contaminate the meth.
Hope this helps all back there in UK.
BAD NEWS TODAY:---- Wife fell over and broke arm in the night and has to have opp in OZ to repair.
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[*] posted on 19-3-2009 at 12:03 PM


Anyone else been brave (read crazy) enough and experimented with demething the whole batch of bio AND glyc together yet?

Did you manage to reverse the reaction and unmake your bio or did it go OK?




DISCLAIMER:
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1992 709D Mercedes
1983 Dodge 50
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1994 Citroen ZX 1.9 TD, Engine now in 1996 Peugeot 306
http://www.biofuel-uk.net/
http://www.biodieselcommunity.org/


GOVERNMENT WARNING!:
If you are having individual free thoughts please switch on your TV immediately and watch x factor, or go shopping, or buy a happy meal, free thought will lead to extremism. It is harmful to the collective good and won't really make you happy. The democratically elected world leaders have your best interests at heart and will do everything within their power to make sure everyone is equal and safe from terrorism and infectious diseases and recession. Please help by consuming as much as you can and following all orders without question!
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[*] posted on 19-3-2009 at 05:25 PM


Hi Chug,

Looking very good, thanks for dropping me a line on this.

If you can do it all quickly and a low temperature, there seems to be very little back reaction, so good on ya!

Nick, I've been away doing other things, mostly cycle racing, so hardly use a drop of fuel these days. Getting the miles in for training uses up most of my spare time (and energy) but none of my biodiesel! I'll never win a race at my age, but I like to pretend I can and do my darndest to. http://www.graham-laming.com/bikes/index.htm

Cheers all, and hope it all works out well for you.

Graham









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[*] posted on 19-3-2009 at 08:28 PM


Hi Graham

did you also get the message about my BBB?

Interestingly, Neutral said it might work better hotter which seems logical, but I don't know how you would do it quickly with low heat?

I'm toying with the idea of demething my next 135 litre with glyc still present, but I may wait to hear how others get on.

Also don't know whether prewash will affect it or not, mine was done without a prewash, so it also needs testing to see if it works after a prewash too, so Nick keep us posted.

Jim
you said you had a batch ready to go and was gonna try both the 2 stage without stage 1 glyc removal and the whole batch demeth, did you try this with your batch yet?

[Edited on 19-3-2009 by Chug]




DISCLAIMER:
Safety is your own responsibility, satisfy yourself it's safe, don't take my word for it!
1992 709D Mercedes
1983 Dodge 50
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1994 Citroen ZX 1.9 TD, Engine now in 1996 Peugeot 306
http://www.biofuel-uk.net/
http://www.biodieselcommunity.org/


GOVERNMENT WARNING!:
If you are having individual free thoughts please switch on your TV immediately and watch x factor, or go shopping, or buy a happy meal, free thought will lead to extremism. It is harmful to the collective good and won't really make you happy. The democratically elected world leaders have your best interests at heart and will do everything within their power to make sure everyone is equal and safe from terrorism and infectious diseases and recession. Please help by consuming as much as you can and following all orders without question!
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[*] posted on 19-3-2009 at 08:41 PM


Sorry Chug, not done yet, been busy sorting other fellow brewers for a couple of days. It looks good for tomorrow, I think I have a clear day.
I'm playing with a small reactor at the moment, 50ltr, incorperating my new high pressure eductor. I'm considering fitting them as standard on my reactors.
If the test model goes well I'll publish the results and design for everyone to have go at.




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[*] posted on 19-3-2009 at 09:20 PM


James, Look forward to hearing how the Eductor works out as I make 50lt batches myself.

Chug, go on give it a try, Iv`e tried both ways with and without prewash worked ok for me.




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[*] posted on 20-3-2009 at 10:36 AM


Hi Chug

No need for the prewash, as you will find that the glycerol and soap separate super-fast as you remove methanol.

The best way to keep temperature low is to ensure the pressure is low, which reduces boiling point of methanol.

Cheers and yes, I'd love to make it to the BBB if possible!

Cheers

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[*] posted on 20-3-2009 at 10:51 AM


I don't understand how the pressure would change from atmospheric in an open sytem like this?

I assume this superfast seperating of soap and glyc is from observations with the HCI acid neutralised demeth?

Is this seperation helped by the acid I wonder? or what I'm trying to say is would the same superfast seperation occur without the acid.

I didn't really notice any superfast seperation of glyc and soap but as it was only a small amount from 30 L batches I just drained glyc into a bucket that already had glyc in it, next time I'll drain it into a clean bucket and observe what happens.

I want to leave the prewash out again anyway so hopefully I get better purity recovered meth.





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1992 709D Mercedes
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http://www.biofuel-uk.net/
http://www.biodieselcommunity.org/


GOVERNMENT WARNING!:
If you are having individual free thoughts please switch on your TV immediately and watch x factor, or go shopping, or buy a happy meal, free thought will lead to extremism. It is harmful to the collective good and won't really make you happy. The democratically elected world leaders have your best interests at heart and will do everything within their power to make sure everyone is equal and safe from terrorism and infectious diseases and recession. Please help by consuming as much as you can and following all orders without question!
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[*] posted on 20-3-2009 at 03:50 PM


The process is underway, I'm going to have ago at all the new ideas in one hit, new 2 stage and full demeth.
I'll report as we go along.




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[*] posted on 20-3-2009 at 09:37 PM


Jim thanks for explaining your processor today. Very impressed.

Cheers for the scrap BTW!:g0180: By the time I had loaded up the other stuff it weighed in just over half a ton £38.

Good luck with the test.

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[*] posted on 21-3-2009 at 09:07 AM


Hi Chug

I was running a vacuum on the tank when boiling off the methanol, to keep the temp low to reduce rate of back reaction.

There is certainly some back reaction, and the hotter you run the de-meth process and the longer you run the de-meth process, in the presence of glycerol and catalyst, seems the more back reaction there is.

You can determine existence of back reaction by looking for presence of mono and diglycerides in your finished fuel, assuming the initial reaction yielded good conversion fuel.

You won't see evidence of the back reaction in a 27/3 test, because biodiesel, monoglycerides and to a lesser extent diglycerides are reasonably soluble in methanol. Tri glycerides don't dissolve at all, but you are unlikely to be making triglycerides in any great quantity in the back reaction.

The simple test I use to gauge back reaction (assuming we start with properly reacted biodiesel ie good conversion before de-mething) is to take the finished de-soaped, de-meth'd but UNWASHED biodiesel, and mix it 50:50 with distilled water. Give it a vigorous shake up and leave for a few hours in a warm place such as an airing cupboard.

This will reveal the presence of mono and di-glycerides, which will tend to form an emulsion layer between the water and biodiesel.

No MG or DG = no emulsion layer.

More MG and GD = more emulsion layer.

No back reaction = perfect separation


The downside for MG and DG being present is an apparent increase in absorbtion of water into the biodiesel, which may increase the risk of bacterial growth, plus an increased viscosity which may be an issue in winter, plus an increased tendency to experience waxing in cold weather. I can confirm that the bacterial growth is clearly evident from samples of back-reacted biodiesel I have in glass jars. They now (after a year or so) have a black slime growing in the bottom of the jar and there are flecks of it on the walls too. - My good biodiesel has no evidence of this.

See how your unwashed but de-meth'd, de-soaped samples perform in the water test.

All the best,

Graham




[Edited on 21-3-2009 by GrahamLaming]

[Edited on 21-3-2009 by GrahamLaming]




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3.Sodium hydroxide/potassium hydroxide/caustic/lye will burn skin. Do not breathe in the dust. Animals will try to eat it as it smells of salt.
4.Concentrated sulphuric acid will burn skin and explode if water is added to it.
5.All these chemicals should be stored properly and kept away from children.
6.Most common serious accident: Processor blows up due to immersion heater being accidently switched on when empty.