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I am somewhat new to biodiesel processing and brand new to this forum. So if I am not clear please bear with me.

I added 93% sulfuric acid (brand new bottle) to methanol and did not get the reaction I was expecting. Everything I read said be ready for a boiling reaction when you add the acid to methanol. All I got was a very minor boil (perhaps a second) and nothing else. At this point I proceeded to add this mix to my oil (which titrated at 9). The oil did not titrate lower after several hrs. and after settling over night I had a separation of exactly the same amount as the methanol I added. I am now thoroughly confused and not sure which direction to head, Any help would be appreciated. Bill
 
Location: yes | Registered: July 16, 2011Reply With QuoteReport This Post
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I'm not sure why the reaction was weak, I had the methanol acid mix boil to the point the whole mess erupted with such force it rose 8 feet out of the container, the splash marks are still on the side of the processor to remind me to never mix acid and methanol. I always add the methanol to the oil, mix, then add the acid.
did you keep the oil hot over night? if so I suspect the oil was wet or the acid was not as strong as stated. How much acid/ltr of oil did you use? To get this bach finished add more acid so that the total acid in the mix is 3ml/ltr make sure the oil is at least 100f and well mixed the let it sit over night (100f - 135f)


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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don't think for one moment that making biodiesel is not dangerous! you should review the AE process discussions before making silly statements. I am offended Big Grin


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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Thanks for the help. The formula I used was titration minus 3 multiplied by .16 I tried heating it and also tried letting it settle over night. I got a separation where the bottom was a murky tan color and the remaining oil was more clear and darker. i am assuming my separation was the methanol I added (the separation was the exact amount of methanol added). I am assuming I should put this liquid back in the reactor before I add the additional acid.
I will try the 3ml/ltr method today and report back. Thanks for all your help. Bill
 
Location: yes | Registered: July 16, 2011Reply With QuoteReport This Post
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NO don,t put that chit back in the processor, murky/tan/creamy colour is an indicator that the oil was wet!, this stuf will be sulfuric acid methanol crap and water. sulfuric acid is a good water mop and drys the oil but at the same time water stops the ae reaction. drainage from DRY oil is black. As you noted the oil in the processor is darker in colour and that is ok. the resulting biodiesel will also be much darker that you are used to from the base or base/base process only.
Just add sufficient acid to = 3ml/ltr in total ( 3ml - your original dose). you can also add methanol at this time but I find that adding acid only works for me, my drainage from a 160ltr batch is never more that 3 ltrs.


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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THank you Thank you Thank you

My first time on Any forum and already you have restored my faith in mankind. I will certainly post my results. Bill
 
Location: yes | Registered: July 16, 2011Reply With QuoteReport This Post



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Hello, it's me again. Home from my 4 day road trip. I titrated the oil in my tank. I mixed it before testing and it still tested at 9. It is very dark in color. Where the heck do I go from here? I started with 35 gal. and am now down to 31gal. after draining the tan colored crud. Thanks
 
Location: yes | Registered: July 16, 2011Reply With QuoteReport This Post
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you had wet oil, that's why the ae didn,t work, if you added more acid as I suggesred above and haven,t drained it out, add methanol equal to the total drainage (4 ltr) then redo the ae. by now the oil should be dry. let me know how you make out. do you have a ph meter? if you do, mix up a normal T sample and check the ph, for ae to work well ph must be 1 or less. this takes the guess work out of how much acid to use.


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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Tom I did add the acid as you suggested before my trip. I have not drained anything since that time. Am I correct that your suggestion is to add the same amount of methanol as I drained out with my tan crud? That would be 4 gal. That would make my total methanol use = 8.8 gal (4.2 initially plus the 4 you are now suggesting) When do I get to add KOH and how much more methanol with that? It looks like this batch could turn out expensive.
I do not have a ph meter. Do you have a suggestion where to acquire one?
I'm not trying to whine and appreciate the help.
 
Location: yes | Registered: July 16, 2011Reply With QuoteReport This Post
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yes add the methanol, AE reuires 10 - 12% dry methanol to work, hard to guess how much methanol was in the drainage. when you do base add the remainder of the methanol as previously calculated. that would be 8 - 10% by volume of oil. There is a prduduct similar to tumeric that will change color at ph 1, I don't have that info with me at the lake but you should be able to find it with a google search.
check this out http://antoine.frostburg.edu/c...old-indicators.shtml


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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Well I titrated the oil I have been working with and it titrated at 6. I figured this was as good as it was going to get. I add 1800 grams KOH with 2.8 gal methanol (my original percentage)Introduced it to my warm oil and crossed my fingers for 2.5 hrs. (man my fingers are sore) I am happy to report that the oil reacted. I did a 27 3 test and it came out super, completely reacted. Doing the wash and dry tomorrow. What a huge relief.
Your assistance has been super. I know I would have never had a positive outcome without your help.Thank you Thank you Thank you.
Now for my next batch of dirty oil would you suggest I use T minus 3 x .20 or 1 ml of acid per liter of oil with 60% of methanol or?????? You are my AE guru. Thanks again Bill
Oh one other question. Can I dry my unprocessed oil the same way I do my finished oil? Heat to 90 degrees and mix it with a fan blowing across for 3-4 hrs?
 
Location: yes | Registered: July 16, 2011Reply With QuoteReport This Post
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yes dry your oil the same way you dry the biodiesel. As far as which formula to use, it is more simple what you are thinking! 3ml of acid/ltr of oil and 1/2 of the methanol you would normaly use for base only processing. Here's the deal, and I've said it before, no formula is going to work reliably for every person because each biodiesel set up is different. After you have completed a few good batches with this acid amont you can start to decrease the amount to determine the minimum amount of acid required for your set up. The down side of too much acid is that water is created when it is neutralized in the base process, the more water = more soap = les yield. Having said that the yied will still be much more than if you had base procssed T 10 koh oil.
If the weather is very humid here oil drying is near impossable, then I use 3ml/ltr, every raction is good. during dryer periods I can get a sucessful reaction with .65 - .75 ml/ltr of oil.
Your ending T is what I would expect useing 3ml acid/ ltr of oil, your yield should be great providing not too much oil was in the drainage.


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post



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Thanks for the easy to remember formula. Simple is always better for me.
I added 10 gals of water for my first wash and ended up draining off 13 gals after an overnight wait. I am assuming that is normal.I now on my 2nd wash and will give you a progress report. Again thanks for your help. Bill
 
Location: yes | Registered: July 16, 2011Reply With QuoteReport This Post
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OMG I can't believe my poor fortune. I bubble washed the second wash and now I have an emulsion. There must be a lot of soap in the method I used,correct? Where to go from here? Wow what a nightmare this batch is turning out to be. Bill
 
Location: yes | Registered: July 16, 2011Reply With QuoteReport This Post
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no big deal Big Grin add 7ml vinigar/ltr of water and stir it in this will break the emulsion, or you could heat the batch that will also help to turn this emulsion back to liquid, many here use rock salt but I'm not sure how much salt they use. emulsions can happen in the first few washes, after that the biodiesel is bulet proof. next batch do a 5% prewash before droping the byproduct this will pull much soap and methanol from the biodiesel. then limit the wash water to not more than 7% of the biodiesel volume for the next two washes, after that you should be good to wash more vigerously.


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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Once again thanks for the help. This seems to be the batch from HE double hockey sticks. I have considered the 5% prewash but I also like to add my glycerin to my next batch. I seem to pick up a 1/2 gallon oil as well as dropping my titration about half a percentage. Will the prewash ruin my chance of using my glycerin in this fashion?
Thanks as always. Bill
 
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Don't pre treat with byproduct if you intend to do ae. this process places toooo much caustic in the oil which will neutralize the acid. everyone needs a batch from -ell, they are such great learning tools Big Grin If you need to keep the byproduct water free drain it the pre wash with 2 or 3 % water keeping the water amount to a minimun will prevent the dreaded emulsion. Tom


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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Hello, I am back. I have good news to report. I tried vinegar to break the emulsion, starting with a small amount waiting for a change and then adding a bit more. After my third small dose with no change I said the heck with this and dumped the remainder of the gallon into the tank. Almost immediately and in front of my eyes it changed, just like magic. It was very cool to watch. I let it mix for a short time and then let it settle overnight. I drained it off in the morning and washed the remaining fuel a few more times. Drained off the water and dried it for 4 hrs at 90 degrees. The bio tested perfect with the 27-3 test. I ended up with 26 gals. of bio after starting this adventure with 35 gals. I am very happy to have ended with ANY good bio. I could have been disposing of 35 gals of crud. Thanks again for you help.
I am now getting ready to AE my 2nd batch of oil. I will be following your advise throughout.
Again thanks for all your help. Don't be surprised if you hear from me again. Ship happens.
 
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congrats, nice result Tom


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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I put vinegar into aqueous potassium soap solution. The potassium went with the acetic acid and left free fatty acids floating on the surface of the water/soap/potassium acetate solution. So in breaking your soap emulsion using vinegar , I think you have probably formed some free fatty acids that are bouyant on the lower phase. If you mix your product biodiesel with hot water, is it neutral? I think there are free fatty acids that went some where.
 
Location: Texas | Registered: April 27, 2011Reply With QuoteReport This Post
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