My first wash. AARGGHH

[Captaincademan Senior Member Find all posts View Profile Close Captaincademan]

Re: My first wash. AARGGHH

I worked out last night that with my particular emulsion, that 4ml of white vinegar coupled with 100 degrees of heat (water was boiling off) was all it took to almost instantly break 900ml of emulsion. the first 2ml made a difference but wasn't enough to completely break it. the second 2ml dose did it instantly.

So the question is, do I need to multiply the sample qty by the size of the entire brew, or just the volume of emulsion? I am thinking the entire brew as it will be evenly distributed (in a perfect world, which we know doesn't exist because there would be a Tilly on every street corner if it did).

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: My first wash. AARGGHH

Hi Cade,

Thank you for your vote of confidence, you have made me blush.

Typically people wash several times before drying.
If you go back and look at the picture I posted of the biodiesel in the bottle sitting on top of white wash water, you could be pretty safe in saying that the biodiesel had only been washed once or twice.
The next thing that would have happened was the water would have been drained and another wash performed.
It is best to try to wash until your wash water is fairly clear. You do not want much of any soap remaining in the biodiesel when you are finished washing.
Then drying should not be a problem.

I Posted the World Famous Dr Pepper Wash Technique (Pat Pend) that describes a method of washing a small test batch of biodiesel that avoids emulsion problems
https://www.biofuelsforum.com/thread...que-(Pat-Pend)

I suggest you try to up-size something along those lines.
I have very few problems when washing when I use that method

[Captaincademan Senior Member Find all posts View Profile Close Captaincademan]

Re: My first wash. AARGGHH

Ok, so after a couple of months of weekends concentrating on a bathroom reno, I am back into brewing again, with a view to making the best possible bio I can.

The old batch mentioned in this post eventually came out absolutely golden, and although it was heartache and tears, I did save it with vinegar, heat and time.

so yesterday I made another batch.

I have installed my u-beaut temperature controller system that I must say is just wonderful. For everyone who heats their brew, This is a superb option. I will try to get some photos and post.

anyway, so sunday morning around 10am I filled the brewer with oil and flicked on the new heater controller, and set the temp to 60 degrees. there is about a 5 degree error in it, I havent worked out how to calibrate it yet.

by 12 it was up to temp and I made the brew. turned off the mixer at 1:30, and let the glycerine settle for about 45 mins.

tapped of the glycerine. Put the garden hose handpiece on 'mist' and timed how long it took to put about 10 litres in a bucket. took about 10 mins.

so I then sprayed 10 mins worth of water on mist into the top of the hot freshly made brew.

gave it an hour or more to hopefully settle. it sure did and water and soap came out the bottom.

turned the heater back on this time set to 95 degrees.

turned off when at temp to stop the convection current.

let it settle for about 10 mins, then dropped off more water.

turned the heat back on and got back up to temp.

turned off and tapped off more crap, but not much this time.

fuel is bright and clear when hot, but still clouds off a little when cooled. I will do one more heat cycle during the week.

checked for water content with the shell fuel tester, and it is a pass. its now 4pm. I am pretty happy that I have made useable fuel in 6hrs.

so - question: based your post above Tilly, do you think I should be doing a second wash cycle, or is bright and clear sufficient? I guess its an easy thing to do to take a sample and see if the wash water is clean?

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: My first wash. AARGGHH

Hi Cade,

... with a view to making the best possible bio I can.

Bright and clear is sufficient for my situation.
The quickest way to determine whether you are satisfied with your wash is to do a couple of mini-washes using the World Famous Dr Pepper Wash technique (Pat Pend)
Once you have finished aggitating, allow it to sit for a bit and see how clear the wash water is
You will be able to see about how much soap is left in the biodiesel and decide whether that is good enough for you.
In my experience, it is very difficult to achieve perfectly clear wash water no matter how many washes you do.

P.S.- You might want to run the mixer at then end of the first wash for a few minutes and gain the benefits available from performing a 5% Pre Wash
While the name is 5%, the amount of water is not critical as long as it is at least 5%

[Captaincademan Senior Member Find all posts View Profile Close Captaincademan]

Re: My first wash. AARGGHH

Thanks Tilly. I will do a little test one night this week.

I should add that I want to make 200 litres of the best possible bio I can in one day.

I want to start making a brew in the morning, and by the afternoon have it ready to burn, with the quality high enough to run it trouble free in a modern common rail.

That's what I am aiming at. I will allow one concession on my self imposed restriction - it can sit in the brewer for a week and be pumped into my storage tanks just prior to making the next batch.

I am very hopeful that I am almost there based on yesterday's success. few little things to work out to streamline the water washing and heat drying, but in essence its all doable.

If i can Reliably make washed fuel in one day with a water PPM low enough to escape detection time and time again, then I will feel comfortable upgrading the ute at some point.

I am really quite excited about it to be honest. strange as I have been making bio for 15 years... !

[Captaincademan Senior Member Find all posts View Profile Close Captaincademan]

Re: My first wash. AARGGHH

So I did the shakemup test for wash water clarity, and it showed a milky white water with a thin layer of soaps sitting on the top.

I then siphoned off the water and soaps from the bottom of the jar, and did a second wash straight away.

it settled out without a soap layer, and the water was lot clearer. I repeated twice more, with no change the wash water colour. (almost clear but not quite).

So reasoned that one more wash was sufficient.

So i brought the brew up to about 60 degrees (wanted to replicate what will happen on the day) and did a second short wash (probably about 5 litres or so on mist sprayed intot he top).

gave that 15 mins to settle and tapped off the bottom.

out came almost clear water then a layer of soapy emulsion. I stopped when the orange juice started.

I then heated brew to 95 degrees. stopped heat cycle and let it settle. out came some more watery bio mix.

kicked the heater back on a ran it up to 100 degrees and held it there for about 30 mins.

turned it off and ran off more watery brew.

now the batch is bright and clear when cooled, and it passes the water test without any hint of water present.

due to the repeated tapping of the watery brew from the bottom I am lowering my yield considerably - probably losing 10-15 litres out of an approximate 190 litre batch. It could also be the residue methanol leaving that is lowering the brew yield.

before I washed my fuel I would usually get around 190 litres yield from 200 litres of oil.

does anyone have any ideas on how to increase my yield? I guess I could then heat the watery brew again and boil off the water to get it back, but thats a lot of energy use in order to get 10-15 litres back.

[Bueff Biofuel Enthusiast Find all posts View Profile Close Bueff]

Re: My first wash. AARGGHH

Hi Cade, brilliant write up, thanks for that!

from past experience, if you let the 10 - 15ltr sit in a bucket until you do the next batch, you’ll find more bio would settle out of the white soapy mix.
That is of course if you have the room or convenience of having a bucket or container sitting around.

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: My first wash. AARGGHH

Hi Cade,

does anyone have any ideas on how to increase my yield?

Instead of turning off the mixer and allowing the glycerine to settle for 45 minutes at the end of the reaction, I would immediately do a 5% pre-wash before the glycerine settles as described in the link in my above post.
This will increase your yield slightly and may reduce the number of washes you need to perform.

I would keep the watery brew from the bottom of the mixer and see how much biodiesel settles out over the next few hours.

[Captaincademan Senior Member Find all posts View Profile Close Captaincademan]

Re: My first wash. AARGGHH

Thanks Tilly.

I read the thread and man that seems counter intuitive, but I will give it a go. seems like an emulsion waiting to happen. I guess the water qty would be less that what I used the first time and created the emulsion which started this thread. 200 L batch would be 12 L of water. I probably used about 18 Litres or so I imagine. plus the glycerine is still in the brew with this system.

I didnt read (or maybe I missed it) how much this early wash increases yield by? or perhaps it is related to the condition of the oil in the first place and it will vary between batches.

do I just dump 12l of hot water in or do I need to spray it in gently like advised earlier in this thread?

Thankyou for your help everyone.

Beuff - I will keep an eye on the bucket and see what happens.

[SUZUDDIS Senior Member Find all posts View Profile Close SUZUDDIS]

Re: My first wash. AARGGHH

Well done Cade. It's been a while but it seems like you have made a gorgeous batch of fuel.

[Captaincademan Senior Member Find all posts View Profile Close Captaincademan]

Re: My first wash. AARGGHH

Hi Michael,

good to hear from you mate. You still brewing? if so I would love to show you my setup now. its quite 'hitec'.. you would love it. I still have your blue drum as well for you.

yes I always aspired to the lofty heights of polished fuel, however it was hard to justify the extra time and effort when I read about all of the bubbling washing required.

this method seems very simple and fast, with bugger all waste water to dispose of.

I keep looking at my sample jars that I heated to 180 degree plus, and then cold filtered, and I cant help but think that method is the absolute bees knees. that fuel is lighter in colour than a bright beer, and as clear as water. very different looking fuel. I will still lend my mind to working out how to do it safely as I dont beleive it requires any washing processes.

all food for thought. but right now I happy to learn this process properly, and get good repeatable results.

side note - it is surprisingly quick to heat up 200 litres of oil to 100 degrees using a standard hot water system as your brewer.

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: My first wash. AARGGHH

Hi Cade,
Yes, the 5% pre-wash is certainly counter intuitive, but it does work- I have done it before when I was water-washing my biodiesel.

The amount of yield gain will depend on the titration of the WVO.

Just a quick explanation.
Neutral performed experiments that showed that for every 1% soap produced in the reaction, the soap will take about 2% biodiesel into the glycerin layer with it.

EXAMPLE
WVO with a KOH titration of 2 equates to the WVO containing about 1% FFA's which, during the reaction will be converted into about 1% soap.
This soap is of course a reduction in your yield in the order of 1%
However, when this 1% soap settles out with the glycerine, it binds with about 2% biodiesel and the biodiesel also goes into the glycerine along with the soap.
You then have a total loss of volume of around 3%, 1% being soap and 2% being biodiesel.
It is some of this biodiesel that is bound with the soap that is released from the soap and returns to the biodiesel layer and so you have an increase in yield.

However, from the reading I have done, it seems that the bigger advantage of this procedure lies in a significant reduction in wash time.
"The concept is that you add water after the reaction is complete, but before settling has started. This helps the settling process, giving a faster more complete settling. Testing has shown a 30% to 50% reduction in soaps in the unwashed biodiesel. I have seen 95% settling in as little as 30 minutes"
http://www.make-biodiesel.org/Biodie...r-prewash.html

[Captaincademan Senior Member Find all posts View Profile Close Captaincademan]

Re: My first wash. AARGGHH

Excellent. Thanks for the good explanation in lay terms. So on the yield side of things I can possibly gain 4 litres of bio from putting in 10 litres of water and mixing for another 20 mins I think it said?

And I can then possibly get away with only one additional wash cycle, or go for the second and get a further gain in quality.

That sounds like a plan.

[Bueff Biofuel Enthusiast Find all posts View Profile Close Bueff]

Re: My first wash. AARGGHH

Hi Michael,

good to hear from you mate. You still brewing? if so I would love to show you my setup now. its quite 'hitec'.. you would love it. I still have your blue drum as well for you.

Dou we have a volunteer and place for our next bio BBQ gathering I wonder???

Cade, I have installed one of these, makes life a lot easier in terms of water amounts

https://www.ebay.com.au/itm/Digital-...QAAOSwq6VcAPfX

I just dump the water in while the glycerin is still in the tank, let the paddle mix for a minute or two and then turn it all off and let it settle, one more wash gives me bright and clear fuel. So far that's good enough for me

Hi Michael, good to see you're still floating around on the forum.

would be great to catch up with you lot again.

[Captaincademan Senior Member Find all posts View Profile Close Captaincademan]

Re: My first wash. AARGGHH

Mate thats very cool. It would be sub zero though if it could close a valve on a preset value!

Me thinks I will get one of those. much more accurate than what I was doing. I am going to order one today. I might see if i can get one that will close a valve though. thanks for the heads up.

Hell I would love to host a BBQ again! not sure how many active members there are around the traps in SE qld / Lismore though?

I better shift this to a different thread. going off topic.