Author Topic: In processor titrated water wash method (Read 109677 times)

Carrington · « **Reply #225 on:** January 07, 2013, 07:56:41 PM »

Hi Dawson
How long are you leaving the water to settle and how long are you mixing the water

db · « **Reply #226 on:** January 07, 2013, 08:24:26 PM »

Quote from: Carrington on January 07, 2013, 07:56:41 PM

Hi Dawson
How long are you leaving the water to settle and how long are you mixing the water

15 min mixes, then 1/2 Hr settle.

If i was short on meth on first stage would this be the reason i used so much caustic? I did dry the oil before use via condenser until no drips.

william crosby · « **Reply #227 on:** January 07, 2013, 08:52:23 PM »

hi

i have found you need to let the water settle for at least 3 hours as it holds lots of bio and you will loose lots when draining water

db · « **Reply #228 on:** January 07, 2013, 09:32:43 PM »

Right that's me done with water washing!!

Tomorrow I'm draining the water, running the condenser and then bubble and settle.

Never again.

Dawson

db · « **Reply #229 on:** January 08, 2013, 08:06:16 PM »

I've dewatered via condensor, taken a sample and done a 50/50 and it's clear. Now to bubble and settle.

I'm wondering if the wash water would not have been cloudy if it it was heated?

Head Womble · « **Reply #230 on:** January 08, 2013, 08:16:47 PM »

Good result.

So are you still done with water washing, or are you going to give it another go ?

db · « **Reply #231 on:** January 08, 2013, 09:19:26 PM »

Hi Mark, I'm not sure.. With the wash water been cloudy every time I can't tell when to stop washing!!

I might try again while I use up the Koh but I've got some ASM comming soon to try which I'm told creates less soap, so hoping to just demeth and settle as normal.

Dawson

nigelb · « **Reply #232 on:** January 09, 2013, 07:17:52 PM »

Everybody's methods are different Dawson and, without trawling through this entire thread to see if I posted the comments I'm about to, I can say that my methods are very simple and effective.

I batched up at the weekend.(150lts).....a bit of a nightmare to begin with as some oily looking water got into the processor. Luckily this time I heated via convection rather than having the pump running. I managed to get the best part of 5lts out by heating to 60C and allowing to settle before moving on to my glyc wash to dry it completely.

I had a good 5/45 after my 2 stage titless process using ASM and pumped to the wash tank after a 7% post reaction wash. I bubble washed with 4 x 10lt washes. 1 on saturday through the night. 1 through Sunday. 1 through Sunday night and 1 through Monday. No settling or stopping the bubbler on any of the washes. By the time I got home on Monday evening the bio was clear and so was the wash water that came out. I heated it all up and did a hot pump wash. Drained that and used the heat to dry through Monday night using my uri geller diffuser. Filtered and winterised last night (Wednesday).

I didn't use any chemicals to neutralise the soaps...just good old fashioned tried and tested methods.

Don't give up on it. Some water washing sceptics have now been converted using the titrated wash method. That carries an awful lot of weight in my book.

Nige

1958steveflying · « **Reply #233 on:** January 09, 2013, 07:28:31 PM »

It's my guess that had Dawson not used the acid wash method that he would most likely of had a massive emulsion on his hands.

nigelb · « **Reply #234 on:** January 09, 2013, 09:16:15 PM »

Quote from: 1958steveflying on January 09, 2013, 07:28:31 PM

It's my guess that had Dawson not used the acid wash method that he would most likely of had a massive emulsion on his hands.

I guess you're right Steve. What I'm trying to advocate here is the need to be careful and gentle when water washing. Done gently, with a small bubbles for the first 2 washes and then increasing the ferocity and agitation in subsequent washes, stand alone washing can be very successful. In all of my posts regarding water washing on this site and the VOD it's what I promote the most. It works...it always has.

I think this titrated acid wash method is fantastic. A real step forward in the removal of soaps in biodiesel. However, it's not something I'll be trying anytime soon for the simple reason that my method works just fine.

Nige

Head Womble · « **Reply #235 on:** January 09, 2013, 09:27:41 PM »

Quote from: nigelb on January 09, 2013, 07:17:52 PM

Don't give up on it. Some water washing sceptics have now been converted using the titrated wash method. That carries an awful lot of weight in my book.

Nige

I was one of those sceptics, I started my bio life using demeth and settle,
I then started mist washing like Nige, but suffered emulsions (probably due to pore convertions).
Now after a few years of going back to demeth and settle I've again gone to water washing, but this time it's the titrated acid pump wash method.

So as you can see I've tried a few different ways to remove the soaps, and I'm now completely sold on washing.

db · « **Reply #236 on:** January 11, 2013, 09:35:29 PM »

I hear ya guys. Like Nige say's, everone does it slightly different and i suppose it's a mattr of try which is best for me. I will try again soon, but I'm hoping with ASM I can demeth bubble and settle due to less soaps produced to start with.

Dawson

RichardP · « **Reply #237 on:** January 20, 2013, 08:01:50 PM »

Finally did a titrated batch, thanks to NigelB getting the bromothymol blue and some of the battery acid.

The oil was dried with the ventrui at 65c then glyc washed. On this batch, 160L, I reduced by base ASM from 3.5 to 3g/l, 2400ml, as I'd been getting 0.7ml dropout after s1 on the 10/90. Processed as normal and got .8ml dropout after s1, used 4.5g/l, 290ml asm, on s2 to a clear pass. (Total of 15.6% meth)

Onto the acid side. Made the titration fluid with 1ml of the battery acid - 1.32sg - to 999ml of distilled water. Titrated both 1ml and 10ml bio samples, and came to 0.2ml/l, so should have used 32ml of the acid. Now this seemed a bit low, after looking at the amounts others were using then I would have expected to use a fair bit more. The acid at an sg of 1.32 works out to around 40% H2SO4, http://www.sulphuric-acid.com/techmanual/Properties/properties_acid_sg.htm

Anyway, as the acid vial was 66ml I threw that all in (didn't want bits hanging around) with 10L of water, pump washed for 30 mins, settled/split very quickly. Another 3 10L washes and the bio tested at 12ppm soap.

Are my calcs right with the acid amount? I'm sure they're ok, but like I said it seems to little for the acid strength and batch size, even the 65ml that went in seems too low, but the results were good.

Maybe it was the base of 3g/l that greatly reduced the need for more acid, as it gave about the same dropout as using 3.5g/l.

Julian · « **Reply #238 on:** January 20, 2013, 08:15:03 PM »

Haven't been through your sums, but with the batch I've just made I used 200ml conc. sulphuric for 80 ltrs of Bio.

nathanrobo · « **Reply #239 on:** January 21, 2013, 12:34:08 AM »

Quote from: db on January 07, 2013, 08:24:26 PM

If i was short on meth on first stage would this be the reason i used so much caustic? I did dry the oil before use via condenser until no drips.

Apologies if somebody covered this, couldn't see it - plus short attn span!

But if your first reaction 'stalled' due to insufficient meth, there may have been excess lye in the fuel. Now you calculate 2nd stage lye on Basis of dropout reading, you now have too much lye in 2nd stage & u have enough soap for bath time :-)

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