Could it be that if you let the byproduct sette for too long the "reactive stuff" has evaporated and/or settled to the bottom of the byproduct container, and is perhaps not used?

Hi all

Been reading the forum for a while now as I'm hoping to start producing Biodiesel within the next few months after much more reading and small scale experimentation followed by the building of a processor.

I run on SVO presently and the idea of being able to reclaim decent oil from the sludge I'm left with due to the cold weather is great news.

Just a couple of questions for High Compression....

Do you have any contact details for the companies willing to take the resulting tallow/glyc mix?

and...

Have you seen this method on Journery to Forever?
Deacidifying WVO
In commercial oil refining this is done with lye (NaOH), which saponifies the Free Fatty Acids, converting them to soaps which can then be removed, but it usually requires a centrifuge to separate it. This is an easier way, no need for a centrifuge.

Use the titration amount of NaOH -- eg, 9.6 grams per liter of oil for our high-FFA 9.6 ml WVO (see above). Mix the NaOH with 40 ml of water per liter of oil. It gets hot. Use a stainless steel container, mix it outside (by stirring), and take care! This is very corrosive stuff, take full safety precautions, have running water handy.

When the NaOH is fully dissolved add the solution to the oil (room temperature), stir gently by hand until thoroughly mixed. Be gentle!

Settle overnight. This leaves soapstock at the bottom. The water stays with the soapstock.

Filter to remove the soapstock -- no need for fine filtering, fine steel mesh will do (like a fine tea strainer). Again, do it gently.

Now process the filtered WVO as usual for virgin oil -- 3.5 grams NaOH per liter of oil, but use 25% methanol, process at 55 deg C (130 deg F), with good and prolonged agitation as usual.

In our tests the product was good, the production rate was 80%. With high-FFA oil like this, it's a a much easier process than the normal single-stage, and it's nice not to have to make such strong methoxide as a straight single-stage process would require with this oil, 13.1 grams of lye per liter oil, or more like 13.6 grams (it needs a bit of excess lye).

It's an alternative -- better than straight single-stage base for oil like this, and while it won't get as a high a production rate as the acid-base method, and it uses more catalyst and gives you more co-products, it's very quick and simple.

This is also useful if you're making ethyl esters biodiesel, using ethanol rather than methanol: the ethyl esters process doesn't work well with oils with more than about 2 ml titration.

As always with a new process, try it first with a small sample, say 1 liter of oil. Be gentle when mixing it -- if you agitate it too much it won't separate easily. If that happens, try heating it, and be more gentle next time.

Would this be an alternative procedure that brings similar results?

Cheers

Yorkshirehobo

Yorkshirehobo-
The idea was to use the byproduct for some useful purpose, and to settle out the tallows to winterise the resultant fuel rather than reduce titration, Thats just a slight bonus.........

Im sorry, I cant take anything seriously from the JTF website--He cant even get the correct base of 5 grams NaOH PL for unused oil right --And please, Don't start me off on the Foolhardy Joke, he keeps promoting!!

mmmm... i sensed a little ill will toward JTF amongst other posts so I'll leave that alone for now. What about the details of companies using the left overs to burn at power stations? Are they still around?

quote:

Originally posted by YORKSHIREHOBO:
What about the details of companies using the left overs to burn at power stations? Are they still around?

Dunno about this but I do know that the glycerol byproduct is usefull to coal producers especially those in AUS the the export to Japan market... I don't fully understand why...

-30°C B100 biodiesel has been produced by Celtic Power in Canada. They mixed B100 biodiesel with Wintron XC30 and then cold filtered fuel. There is a mention of this on the Biofuel Systems website (http://www.biofuelsystems.com/wintron.htm)
Has anyone else tried this technique?

Update to my post on page 6.

I tried heating the cruddy oil/glyc by product by standing it next to a radiator, Nothing. So I heated it to 50°C and stirred it a little and then left it to settle, upon checking well over a week later I had less good clear oil compared to what I started out with and the rest is almost a lump of gel.
The glyc by product I used is NaOH base and was pure glyc with no added water from glycwash/prewash, I also had a friend try this using some of my glyc by product and he said he got similar results basically ending up with a reduced anmount of usable oil, I have no doubt that some people are getting a result with this method it's just that so far I have not, I will have to wait a while before I can attempt this again as fortunately most of my oil is good and it takes time to for me to accumulate the cruddy dregs.

Anyone got any before and after pictures?

Chug

quote:

Originally posted by OB1 CANOLA:
well i have to say something for time with this process.After mixing in the koh glyc I let this oil settle in the barrel for about 7 days.
The wet oil had separated and i had nice clean oil on top and a whitish(beige) glop on the
bottom about 3 inches. (this was about 15 gallons of oil in the barrel) The oil was somewhat clear but not really clear.The oil was also less viscous.Which says to me that there may be some partial conversion going on here. It titrated at 3 this oil usually titrates at 4 to 5.
Again leading me to believe there may be some partial conversion. I am processing it right now and will drain the glyc in the morning.

The big thing..As i said above.. this oil was
signifacantly wet as the top blew off the 55 barrel outside the restaurant during a storm
2 weeks ago.The oil decanted off the top was dry.
I put about 2 gal in a pot and brought it up to
250 f and not a pop. This may prove to be a less NRG intensive way to dewater oil. Can't wait to freezer test this batch.
If I do this again i may try to filter the glop
and make soap from it .

Well i am washing this batch now
I think neutral got it right about the reduction in titration amount due to the remaining lye
in the byproduct neutralizing the ffa.
this oil did seem less viscous after it settled
though.

quote:

Originally posted by Old300D:

quote:

Originally posted by Old300D:
I have recently come into a partially hydrogenated oil source that titrates at 5 grams KOH, and have made a 1 liter sample. I then took the glycerine by-product and treated another liter of this creamy glop with it. I got a nice separation, and a layer of crap about as thick as the glycerine. My next step is to make another 1 liter batch with just the top oil and compare the two batches of biodiesel. Should be interesting.

And interesting it is. I took the oil off the top. It titrated at 1 gram KOH. I only had 1/2 a liter, so I took 100ml methanol and 1/2 gram KOH, and made a 1/2 liter test batch.

No separation. As far as I can tell, I have no biodiesel to test against the original test batch. I will try again when I have some glycerine by-product. Very strange, I've never had a test batch not separate before.

OK. As harry747 pointed out I only added enough KOH to neutralize my FFA. I mixed 3.5 grams more lye to 50ml more methanol (1/2 liter batch) and the mixture separated. It is now washed and dried.

So I took a sample of biodiesel made with the "FryOn", a hydrogenated corn/canola fryer oil that titrated at 5ml KOH, and a sample of biodiesel made from the top oil treated with the glycerine by-product (no water) and settled. Both samples filled to the same level in identical containers.

Since I don't have a good way to set cold temperatures, I decided to freeze both samples, then thaw them together at room temperature while I watched. This should give some idea of the temperature characteristics relative to each other. And what I observed was the samples thawed identically - no difference. No apparent difference in cloud point or pour point.

For the record, the glycerin byproduct I used was fresh.

quote:

Since I don't have a good way to set cold temperatures, I decided to freeze both samples, then thaw them together at room temperature while I watched. This should give some idea of the temperature characteristics relative to each other. And what I observed was the samples thawed identically - no difference. No apparent difference in cloud point or pour point.

I have to concur.After my glyc pretreat
my biodiesel reacted identical to a batch i had made pryer. same cloud/gel point and melting point.
I do like how this dewaters the oil though.

Bump--Had a PM on this subject....Hope you dont mind the bump....

I have a couple of questions about the glycerine pre-treatment.

1. It seems like the jury was out, at least as of Sept. 2005, as to whether this would work well with KOH-based glycerine. Is there any update to that?

2. It sounded to me like the separation process took a long time...on the order of several days. None of the experiments I heard about had a control where un-pretreated oil was allowed to just sit for the same period. Is it possible that just sitting without pretreatment might have the same effect?

3. My collection barrels are open-top barrels with a removable lid. I then pump oil from the top of the open container into one on a trailer. Has anyone tried this pretreatment where you just dump the glycerine into the empty barrel and leave it at the restaurant? The oil would be added in doses over the course of the next week or so, but it might save some time. If the methanol in the glycerine is important, that will have a good chance to just evaporate away. Any other drawbacks that you can see which are obvious?

Thanks...

my results with this were mixed . I used koh.
cloud point was about the same with the bd as it was in batches prior that i didn;t do this to.
It did seem to dewater the oil nicely.
in subsequent batches it did not seem to work on
hydrogenated oil that was at room temp and slightly gloppy. All in all it was an interesting
experiment and worth furthur investigation when 'i get up and running again.

quote:

Originally posted by OB1 CANOLA:
my results with this were mixed . I used koh.
cloud point was about the same with the bd as it was in batches prior that i didn;t do this to.
It did seem to dewater the oil nicely.
in subsequent batches it did not seem to work on
hydrogenated oil that was at room temp and slightly gloppy. All in all it was an interesting
experiment and worth furthur investigation when 'i get up and running again.

Hmmm...has anyone processed two batches from the same feed stock, one with KOH and one with NaOH and compared them on gel temperature?

I have a revised process for the addition of the glycerine....

Ive been doing some experiments lately with the real cruddy oil/tallow/water and other hideous stuff left in the bottom of cans/cubies we get at work...

All the 'good' oil is transferred to the main tank ready for the reactor. The dregs, including water, food, chips, snails, dead-rats and mostly the sloppy tallows etc get roughly strained into the 'gloop-tank'. which is around 1000 L capacity. This gets pumped into an IBC, and then the glyc is added...

The usual way was just to stir it in. but lately Ive been having great results by 'spraying' the glyc into the IBC, directing the flow over all the surface as much as is possible, and at some pressure from a hose powered by a pump from the meth-recovery unit. The glyc is usually fresh, and still hot, around 40-50 degrees C, before the meth has been recovered...

The IBC is usually filled to around 900 litre level with cruddy oils/some water and only around 50 litres glyc added--The secret seems to be that the glyc is directed over the whole surface as much as possible rather than the quantity used...

I found that it doesnt need half as much glyc to get the job done, and quite often will 'recover' around 50% or more of the volume of crud in good usable oil, the heavy whitish tallows settling and left in the IBC for disposal to the anerobic-digester guys who love the stuff....

The settling of the tallows seems much faster, and is mostly done in 24 hours, the 'recovered oil' then ready for the reactor.

As usual, Im using NaOH, with an average of 8 grams per litre in the reaction, and 20% meth...

quote:

Originally posted by Boss:
Do I need to find a conversion program to convert these results from Centigrade to Fahrenheit, or can you get me close enough?

Just in case anyone needs this:

Conversion Website

-Jim

quote:

Originally posted by High Compression II:
The usual way was just to stir it in. but lately Ive been having great results by 'spraying' the glyc into the IBC, directing the flow over all the surface as much as is possible, and at some pressure from a hose powered by a pump from the meth-recovery unit. The glyc is usually fresh, and still hot, around 40-50 degrees C, before the meth has been recovered...

Kind of like mist washing...just using hot/warm glyc.

Unlike water, the glycerine does not settle out cleanly to the bottom. You cannot suck from the bottom and use it to mist wash again.

-Jim

So when we pre-treat WVO with fresh by-product from a previos batch we are:

1. Causing a partial reaction.
2. Turning some FFA's to soap.
3. Droping out water/ other suspended particles.

If this is the case. How much methanol remains in the newly settled glycerine layer?

Would it be wize to add koh to the fresh by product and get more FFA out of the low quality oil?

In another direction , could you add methodoxide to fresh by-product and use it in your processor with dewatered wvo? Obviously you would need to know how much koh was in the byproduct. We already know that about 2/3 of the methanol is in the byproduct layer. But how much koh is in there?

There is a residual catalyst test that you can do. I think it is described at www.biodieselcommunity.org .

-Jim