I hav ejust started making bio and the first batch looked great accept it had a very small cloud of somthing that settled to the bottom after a small amount of time, ( I put a small sample in a 20oz bottle, it was quite clear but after a couple of hours I can see a somthing at the very bottom?. I was told i did not dry it enough by a guy that looked at it. The minute amount did not bother me to much so I put the 10 gal batch in on top of 20gal of #2. The next 10gal batch got started and when it cam to drying I ran the heat at 125 deg and after two hours took a sample in a masson jar and it looked very cloudy. I then continued the drying for another 2 more hours. At the end of this I pulled another sample in a jar, still cloudy. I let the jars set over night. The cloud settled to the bottom. the jars have about 4inches of bio, and out of the 4 inches the bottom 1 inch is a cloud ( the cloud looks like cotton balls in the fuel to give you an idea). Both batches titrated out very low, 1st 2.25ml and the second 1.5ml. I am using a 3.5 as a base and 21% methanol. Any help would be great. I do not think its water. I am leading towards an incomplete reation???

General consensus on this and many other forum is that the 3.5g base (NaOH) is not sufficient. Increase that to 5g+titration amount. This would also point to the incomplete reaction you suspect.

Yep, I would agree that it's incomplete reaction problems. As someone who used the 3.5g/L from JtF for a month, it's too low. When you're using small batches, the small amount of excess used is sufficient to make up for the low amount in the base amount. However, when you get to large batches (50L for my first one) it's not enough. Mine emulsed horrifically. Had to quench with all sorts of tricks.

However, 5g/L is now accepted, as stated and I was recommended since it's better to have a little too much than not enough, multiply your titration amount by 1.1.

I wanted to add that the second batch was reacted at over 225 degres, only because I dewatered and add the oil straight to my reactor. So lets say it is an incomplete reaction. What next do I do to this very cloudy batch? Can I add a small amount of meth and lye to clear it up? If so how much meth and how much lye?

Pakhvan, I agree with the others that your NaOH base amount is too low.

I will recommend though that you think about using KOH (potassium hydroxide) instead. It's base is 7.7 g/L but it's very tolerant of mistakes and will not form a solid if too much is used.

What can I expect if I run this batch that may not be completly reated? Can it be saved? Is it junk? If I should have used a 5.0 base can I add the missing 1.5 grams of naoh per ltr to 5% meth and rereact. I am up for any sugestion but would love to work with this batch not for the fact that I will be out the $ if I toss it, more the info I will learn by fixing it.

quote:

Originally posted by pakhvan:
What can I expect if I run this batch that may not be completly reated? Can it be saved? Is it junk? If I should have used a 5.0 base can I add the missing 1.5 grams of naoh per ltr to 5% meth and rereact. I am up for any sugestion but would love to work with this batch not for the fact that I will be out the $ if I toss it, more the info I will learn by fixing it.

Fudge to the safe side. Use 10% methanol and 2 grams of lye. You said previously that you reacted at 225 degrees? That will boil off the methanol and starve the reaction. Methanol boils at 148.5 degrees, that is why so many people recover excess meth, it is pretty easy to get it condensed. The batch is definitely salvageable and will make good fuel.

Norman

thanks for all the help and sugestions. I will try the 10% meth and 2g of lye and post the results. Any other sugestions are always welcomed.

well?? I put in 10% meth and 2g of lye per ltr. I now have ?. It looks the same as before but much more of the thick cloud at the bottom. I also notice that at the top it builds a thin lawer that when pulle to the side with a stir stick another lawer forms almost instantly? As the lawer builds at the side that i move it to it has become a spot of gel like substance about the consistency of well the consistency of snot. Not sure what to do next. At this point I am wondering if the first reaction process was over reaction instead of under. I know that it may be many issues and variables but any ideas and help would be great. Keep in mind this was my second try at this and the first was almost perfect. If anyone wants to call and chat my hm # is 503-667-9272 Paul my location is Gresham Oregon.

I reprocessed the entire batch with 2g of lye per ltr and 10% meth as on person recommended and crashed the entire batch. I drained the reactor and am doing some test batches ( 1 ltr each ) to learn what happened. I may post my tests and results.

final analysis. I ran four test batches on 4ltrs of oil. The oil titrated at 3ml. I used four containers with 1ltr in each. one with a 5grm base, one with a 3grm base. another with 1.5 grm under the 3.5grm base and the last with 1.5grm over the 5grm base. This gave me four batches ranging 9.5, 8, 6.5, & 5grams of lye per ltr of wvo. The end result was very interesting and I believe that the 10gallon crash was due to the excess temp of wvo when reacted. As mentioned I dewatered and added straight to the reactor, added methoxide, and cycled the pump. Not one of my 1 ltr test came even close to the 10gal crash. I thing the methanol boiled off before the reaction got the chance to use it.

Just to be clear on this, did you find a process description somewhere that said to process at that high of a temp.

If you did please post the site so people can be warned of the mis information.

NO! this high temp mistake was all mine, and I believe it to be the reson for what took place.

quote:

Originally posted by pakhvan:
NO! this high temp mistake was all mine, and I believe it to be the reson for what took place.

Well, you are not alone.

I just posted a couple of photos of my experience with soap formation. I reacted in unsealed vessels, AND, I let the temperature get too high.

Does your BD/soap look anything like this?
http://biodieselpictures.com/viewtopic.php?p=762#762

After recovering from my methanol vapor induced headaches, I learned that the reactor vessel, no matter what the size, should be sealed, but not pressurized. I also learned, as a practical matter, that one should not let the reaction temperature exceed about 65C.

Yes that looks very similar. See if yours gets a skin on the top that when pulled to the side a new skin forms. The skin is amber in color just like the bio would be. I did find that after sitting some (possible usable) bio came to the top when left in closed containers. I ended up scraping the whole batch.

quote:

Originally posted by pakhvan:
See if yours gets a skin on the top that when pulled to the side a new skin forms.

Been there, done that too.

Look familiar?
http://biodieselpictures.com/viewtopic.php?p=763#763

I agree with Raften----don't react with the temp that high again. You're asking for trouble. As others have mentioned---use more catalyst. Stuart