Author Topic: In processor titrated water wash method  (Read 109682 times)

Offline Chug

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Re: In processor titrated water wash method
« Reply #165 on: November 04, 2012, 06:23:28 PM »
I'll see If I can find any of the discussions on neutralizing the remaining catalyst from push n pull processor and my early wbd trials,  some folks in US still do it before they wbd as standard as they got used to it from their push n pull days

looking for more on this and remembering it used titration of the whole batch with phenolpthalein for accuracy over sample titrations and added HCL acid until colour change on whole batch,  I'll have to find it now as it's got me head going.
« Last Edit: November 04, 2012, 06:43:01 PM by Chug »

Offline Tony

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Re: In processor titrated water wash method
« Reply #166 on: November 04, 2012, 06:42:58 PM »
I'd be very interested in that Chug.

Offline 1958steveflying

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Re: In processor titrated water wash method
« Reply #167 on: November 04, 2012, 07:04:05 PM »
I'd be very interested in that Chug.

Me too.

Offline Chug

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Re: In processor titrated water wash method
« Reply #168 on: November 04, 2012, 07:08:02 PM »
searching through old stuff I've found it was 34% concentrate HCL and my notes say approx 100ml per 100 litre batch but gotta go have a sarnie or summit so I'll be back on the case in a bit
« Last Edit: November 04, 2012, 08:23:09 PM by Chug »

Offline Chug

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Re: In processor titrated water wash method
« Reply #169 on: November 04, 2012, 08:22:57 PM »
Right I've found some info posted by GL, obviously it was for neutralizing catalyst before demething the whole batch, but it should neutralise soap and instead of demething you guys will then just drain glyc and water wash instead, or maybe even experiment and try water wash with all the glyc in, obviously no good if you need it for glycwashing though

*****************************************************************************
Hi GM

As Nick mentioned, the viscosity rises dramatically as methanol concentration in the glycerol drops, so the venturi fails to operate if using glycerol alone..

So here's an interesting twist, which works well, I have had no issues with back reaction as far as I can tell, and no problems with foaming....

After reaction, keep the pump running and do NOT drain the glycerol, and do NOT do 5% prewash,.

Instead, add a 1/2 teaspoon of phenolphthalein powder per 100 litres batch and allow to mix thoroughly. You'll need a sight tube to view the mixture. A narrow clear branched tube, off the outlet of the pump is safest - you want to be able to instantly see the colour change, so the tube must carry some of the pump outlet flow thru it.

Very slowly (I mean VERY SLOWLY) dose 34% conc. HCl into the inlet of the pump and note the colour change. When you get to about 0.1% dosed volume, you'll see the deep red will lighten up a bit.

STOP adding HCL at this point.
The colour will darken again in a few minutes, DON'T add any more HCl or you will start to make FFA from the soap. The lye will preferentially neutralise first with the HCL, then the soap.

The NaOH or KOH should mostly be neutralised now, making it an ineffective catalyst for what follows...

Add heat to the whole batch and start distilling off the methanol, you'll need to go up to 90C or more.

When this becomes a trickle, stop.

The glycerol will drop out within a matter of seconds when you stop the pump, drain it before it cools and solidifies.

Then drain off the remaining biodiesel into a settling tank to allow soap to drop out, or you can wash it gently as is - it should wash fairly easily if you treat it gently for the first one.

Key things
1. Use a pump which can deal with the viscosity.
2. Don't OD on HCL.
3. Don't dose HCL too fast, or you'll make FFAs

For a 100 litre batch, you'll use around 100ml HCL, depending on titration, amount of lye, water in oil etc.

My pump is roughly 1/2 batch volume per minute.

Dose the HCL at a rate which will take around 30 minutes to complete, at the inlet of your pump so it mixes well.

This is info to the best of my knowledge to date - there is a lot still to learn and much can be done to improve the process, but it is showing good promise as a simple, fast efficient way to recover methanol from the whole batch and aid washing or eliminate the use of water.



« Last Edit: November 04, 2012, 08:38:08 PM by Chug »

Offline Tony

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Re: In processor titrated water wash method
« Reply #170 on: November 04, 2012, 08:44:47 PM »
Best bet for WBD is to use 96% Sulphuric (which I'm currently trying to find at a reasonable price) and then titrate for neutralisation before demething.  Adding water in any form sounds like a bad plan for recovered Methanol quality. Question is how to titrate bio+glyc?

Offline nigelb

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Re: In processor titrated water wash method
« Reply #171 on: November 04, 2012, 09:02:35 PM »
What's the best price you've had for the Sulphuric Tony?

Nige

Offline Tony

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Re: In processor titrated water wash method
« Reply #172 on: November 04, 2012, 09:04:22 PM »

Offline Carrington

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Re: In processor titrated water wash method
« Reply #173 on: November 04, 2012, 09:10:31 PM »
I haven't tried to titrate bio and Glyc yet but I would assume that taking a sample while the batch is mixing then  drawing 1 ml straight away and dissolving ipa should give close indication.

I'm going to try some test batches tomorrow if I can with some new oil .
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Offline Chug

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Re: In processor titrated water wash method
« Reply #174 on: November 04, 2012, 09:27:48 PM »
yeah I think a standard ipa titration should work too

Offline Head Womble

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Re: In processor titrated water wash method
« Reply #175 on: November 04, 2012, 10:06:18 PM »
Umm, I wonder if this could help with HMPE formation when WBD is combined with non titration method.
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Offline Tony

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Re: In processor titrated water wash method
« Reply #176 on: November 05, 2012, 08:02:41 AM »
Add titration to the non-titration method?  Burn the heretic lol!

Seriously though, sounds like a plan to me.

Offline Carrington

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Re: In processor titrated water wash method
« Reply #177 on: November 06, 2012, 04:58:37 AM »
I haven't tried to titrate bio and Glyc yet but I would assume that taking a sample while the batch is mixing then  drawing 1 ml straight away and dissolving ipa should give close indication.

I'm going to try some test batches tomorrow if I can with some new oil .

Well got flooded out in the factory over the weekend so spent a lot of yesterday mopping up , will try and make some hmpe's later in week
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Offline nigelb

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Re: In processor titrated water wash method
« Reply #178 on: November 24, 2012, 06:51:52 PM »
I've been to see Keith and Lorretta today to drop off some winteriser....I also dropped off some battery acid I got from work. Brand new and sealed in seperate vials. These are available to anyone passing their door...FOC. It will save you the bother of using acetic acid (vinegar). I think it's 1230sg

Anyone passing my door in Leicester can also have some FOC...but I'm not going to post any. Sulphuric Acid through the post does not sound like a clever thing to send.

Nige

Offline nathanrobo

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Re: In processor titrated water wash method
« Reply #179 on: December 22, 2012, 03:55:19 PM »
Has anyone discussed the water method of testing prior to pump washing?  I couldn't see it but it's a rather big thread now.

I done this on a few batches now, after each first test I get cloudy water drop out and then continue to add acetic acid until I get a a clear test. 

I had been transferring the fuel to my wash tank before adding water via a hose pipe and pumping.  The last time, I just sucked in the water via the pump's suction on my processor, I settled for 45 minutes each time under heat and got a good split.  In all I reckon 30 - 35 litres.  Perfect 50 / 50 clear.

Question is, are there any reasons why this slight variation is a bad idea?