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John H
12th August 2006, 07:06 PM
Hi All,
I got some WCO from a take-away shop only a couple of sample bottles and looks like it may be no good.

The WCO appears to be shortning/animal fat and soildifes at room temperature, comes in cardboard box with red writing. Oil is changed every week according the the owner, wehn I was there the previous Friday they were changing it, and it was changed this Friday.

Made up the titration fluid 1g KOH to 1lt of demineralised water OK,
did a blank tritation like Tilly showed us at Peda's, 10ml Metho, end of a tooth pick of Tumeric and mixed, 1ml of the WCO microwave until first bubble, mixed with chopstick and dropped in the titrate solution it took
9ml. Caluclated it out Base of 7.8 (90% KOH)+ 9grams = 16.8 g seemed like a lot? Did a 1 lt test batch with 220ml methonal no good at all.

Did another tritation using Phenol Red (from pool shop) this measured at 8ml. So my thought is the oil my be no good.

Any help would be appreciated or am I doing something wrong.

Regards,
John H

Matt
13th August 2006, 02:53 PM
Hello John,

oil sounds like its high in FFA so if your game do a 1 litre test batch, heat to 55 C and add 80ml methanol mix and then whilst stirring add 1 ml 98% sulphuric. Mix periodically over say 6 to 12 hours, then titrate the oil it should come down to well below 10 perhaps 5? or lower. 24 hours may help out too but its hard to stir when sleeping! It may be better to try 2ml acid as a start point but this will raise your endpoint titrated value (Titration done before adding base catalyst) . I use 1 ml acid and get an endpoint of 1.5 (NaOH) which is as low as it can go.

I allow for this in my base stage and use KOH ending up with approx 10 grams per litre of oil.ie. 7 start plus (1.5 times 1.4 to allow for NaOH to KOH) divided by 0.9 to allow for purity of the KOH. (Actually this is 10.11 but its close enough)

Its worth trying you may well make a fuel more than suitable for most of the year in Qld.

Matt

John H
13th August 2006, 07:59 PM
Hii all,
Thanks Matt
I will pick up some sulphuric tomorrow and give it a go, I will let you know how it goes.
Might be off the Internet for a while though as our computer is not booting up windows correctly, windows message said 'recovering from a major error' had to go to Norton Fix, windows had 84 errors, I will ring the man tomorrow. Once I get it going it seems OK.
Regards
John H

Matt
13th August 2006, 08:10 PM
Evening John, funny we should be talking bio and acid base processes and at the same time computer issues.

I finally have had a gutfull of windows and this is from my new Linux workstation, wow what a treat it was to setup. Ubuntu on my AMD64, no reboots at all.

Anyway go on over to the infopop forums and do a search on the FATTA method it will give you the full process its not too hard. The only thing is the acid stage will produce water, in your case more than I get in mine as your starting titration level is far higher, so it may produce a bit of soap in the base stage be warned. The only way around this is to remove the acid/methanol/water phase and start with a new 20% dose of methanol and catalyst. Its apparently not too hard but when it all scales up its another matter to try and do it from the system when your making 100 or 1000 litres of the stuff.


Regards indeed, you're a new/acid base producer, well that all depends on how it goes.

Matt

Matt
13th August 2006, 08:15 PM
Sorry John I just read my first reply and reailised that I did not finish the whole process for you. After the acid treatment we add the remaining 12% methanol with the required amount of catalyst as determined by a titration, called the endpoint titration after the acid stage.

Anyway try it out and let us knwo how it goes.

Regards,
Matt

John H
14th August 2006, 08:05 PM
Hi All,
Thanks Matt for the extra information.
Show holiday up here today, chased around but no luck finding sulphuric in this area, I will have to go further afield on my next RDO.

Just at the end of 2 weeks holidays, did a little more work on my processor but as usual it has had to take a backseat as I have been preparing the area (paving and underground pipes) for rain water tanks and pump, tanks arrive next Friday.

The computer man is not coming until next Monday and the only way I can get the computer to work is do a Norton Windows fix each time and then wait & wait until it loads up, everthing I know about computers you could write on the back of a postage stamp with a felt pen.

Regards and thanks again,

John H

Matt
14th August 2006, 08:40 PM
Goto the Brisbane suppliers page and you will see that Industrial Cleansers at Bilsen Rd Geebung do sell it, a bit of a trip for you but at least its northside.

Matt

John H
8th September 2006, 05:49 PM
Hi All,
Matt
Last week I purchased some Sulphuric acid (Electro plating shop 98%). Last weekend I mixed 1Lt heated UCO, 50Ml Methonal, sturred,added 1Ml Sulphuric, sturred over the rest of the day and let sit until today, Friday.
Titrated at 1 (one), mixed methoxide 1+7.8=8.8g KOH, 200Ml Methonal, oil at 55C, perfect reaction and separation, mixed at 15 minute intervals for 1 hour.
After 2 hours I have about half Bio diesel and half glycerine. Would you think that would be about right. I will measure the amounts when I separate and before washing.

Thanks Matt
Regards John H

Matt
8th September 2006, 09:13 PM
John, it does sound a bit odd that its approx 50/50 bio/glycerol. Your titration at 1 is also odd as the acid should give an end point titration of 1.5.

I would suggest you check the titration process in all aspects. What was the starting titration too? I can only think that this is the cause of such a disparity.

I must admit my process is now a recipe as the oil is constant and we get very good result using the same formula as you. Only difference is we use 80ml methanol per litre of oil int he acid stage, then the remaining 120ml methanol per litre of oil in the base stage. 10gm KOH per litre of oil and hey presto add heat and stir.

Might pay to try another batch?
Matt

John H
8th September 2006, 10:16 PM
Hi all,
Matt,
Yes I will do another batch and cross check the results but at least this time there was a reaction.
I will keep you posted.
Thanks
John H

Matt
9th September 2006, 09:35 AM
John, just reread your post and I noticed something I should have picked up last night. You say that you left the acid stage to go for about a week?

If so this is too long, I have read that leaving it go after the lowest titration value it gets to will cause it to rise again. Not quite sure of why as a few have theorised and I am yet to read anything definitive from a reputable source. Needless I believe it will, why I am not sure.

SO do the acid stage for a max of 24 hours. Depending on the titration of your starting point you will only go so far. The amount of acid may increase slightly to say 2ml per litre but this is for nasty oils. If yours is reasonable at the start then 1 will do the trick and bring it down to a reasonable value. Again titrate at the start, put in methanol and acid and stir. Each hour stir and titrate. Stirring is critical as the methanol and oil have different SG's and will seperate and how will you make methyl esters if they are seperate? MIx well and often. When the titration has do the dropped and is not changing then then do the base stage.

Hope this makes sense, if not yell for more.
Matt

John H
9th September 2006, 07:49 PM
Hi All,
Matt
I measured the results of Batch No 1, 700Ml of Bio and 600 Ml of Glycerol total 1.3L. So I have 50Ml more than I started with. I think I must have been more than gernerous with the Methonal. I remember using 80Ml in the acid stage then still added 200Ml at the second stage so I gained 20Ml somewhere? (Bad measurements I guess). Also was a bit lost, in an earlier post "add the remaining 12% methonal" but a later post 120Ml .

The Bio is very light in colour, just a little darker than the batch I did with new oil and the glycerol is the colour of light honey. I am in the wash process with it now.

This Oil Tritates at 10g per litre.

Started Batch No. 2 this afternoon after the first hour titration was 9g
I will reheat and Stir, stir in the morning titrate and possibly make batch No. 2 in the afternoon. I am certainly learning a lot thanks to you.

Regards
John H

Matt
11th September 2006, 10:41 AM
John, certainly sounds like too much methanol in the first batch, this will account for the funny ratio of bio to byproduct as the excess methanol will reside in the lower layer.

Do your batch with the oil starting at 9, mix as I said and titrate periodically, you are looking for the lowest point it will reach as shown by repeated titration. Then do your base stage using this titration value. It includes the acid you added so all is fine just add it to a KOH base of 7 and allow for purity of the KOH. Mind you I find a fair amount of soap in my fuel so I am looking at dropping out the purity adjustment as some people have said it may well be made up of NaOH anyway. Worth a try.

My current batch started to soap up immediately I turned on the sprayers, so I heated it up and drove off the methanol and started again and since the liquid was hot (60 degrees) and the water would be warm it went well.

Dried it yesterday will decant today, I need fuel!

Matt

John H
14th September 2006, 08:21 PM
Hi all,
Matt
Thanks for the reply, the computer has all but given up, took it to the 'MAN' Monday and got it back today can't fix it, so now I am computer shopping.

Batch No.1 I tried to take a picture of the result so I hope I can attach it. It has been 6 days since the finish wash.

Batch No 2 I think will be a failure it is still solid I ran out of time last weekend.

So here goes with the attachment.

Sorry Matt file size was 749.0 kb can only upload 125.0 kb on the forum don't know what to do to get it smaller.

Regards
John H

John H
14th September 2006, 09:35 PM
Hi All,

Try this link to Photo bucket.
http://i93.photobucket.com/albums/l62/JohnH_1/IMG_0011.jpg

Hope it works, there must be a easier way?
Regards John H

Matt
14th September 2006, 10:22 PM
Words cannot describe, its beautiful!

Superb fuel, go and put it in the car now!

Matt

John H
15th September 2006, 05:49 PM
Hi all,
Thanks Matt, It looks good to me also. Now all I have to do is replicate it with small batches and then upscale to usable quanities. Keep your fingers crossed.
Ordered a new computer to day delivery late next week. Friday we go with caravan club to Canungra (show grounds) for the weekend, probably set it up after that.

Regards
John H