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can't get AE to work on 40 gal.wvo
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Have 40 gallons of wvo in reactor that titrates 15 .I did a 1/2 liter test last week and got it to drop from 15 to 5 in 36 hours .This batch in the reactor isn't changing after almost 3 days. I turned the heat off after 2 days because it wasn't going anywhere. I used 2cc.of Rooto/with 70cc. methanol per liter. Test sample was a half liter ,so I used 1cc Rooto with 35 cc. methanol,and it worked. The sample test was in a sealed jar ,placed in a 130F water bath . I don't know what went wrong.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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hetabeater
-rooto is that drain cleaner or straight sufuric acid? it must be 93% minimum.
-AE doesn't work for one of three reasons loss of heat, wet wvo and caustic resadue in the processor. you can overcome the latter two to some extent by adding more acid, you shouldn't need anymore methanol. If the T hasn't dropped in say 12 - 14 hrs, IMO the reaction is dead. 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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What do I do? Should I bump up the amounts and start over again?I think I might have lost methanol out of the vent pipe. Tom,like you told me earlier, the vent pipe should be long enough so the methanol will condense and drain back. Could I have lost enough with temp running 130 F,to stop the reaction process? Orginally the sample jar wvo was heated and the acid and methanol added ,but the wvo cooled down and after about 12 hrs. showed no response either. But after 12 hours or a little more in the 130 F water bath the reaction really responded. It wasn't even stirred up that much.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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Originally posted by heatbeater:
What do I do?


My advice is to use sulfuric acid. Rooto is NaOH crystals, Rooto liquid Drain cleaner is also NaOH premixed, neither contains sulfuric acid.

Norman
 
Location: Lincoln, NE | Registered: April 10, 2006Reply With QuoteReport This Post
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According to the MSDS Rooto sulfuric drain cleaner is 93.2% sulfuric acid.
 
Location: Southside | Registered: January 12, 2010Reply With QuoteReport This Post
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There is the alkaline (or lye type) and the acid type of Rooto drain cleaners.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post



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According to the MSDS Rooto sulfuric drain cleaner is 93.2% sulfuric acid
HI South,is that what you use for AE?
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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I just stirred up the 40 gallon batch and took a sample . A titration says its 10. I'm going to put a half full jar of it in a warm water bath (130F)for 12 hours or so and see if responds .If it does, than that tells me there's enough methanol and KOH in it and it just needs more heat. If it doesn't respond to any heat ,my guess is to start all over. I'll post the results within the next day.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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Heat beater
-drain a ltr from the bottom, tell me what you see, is it black or does it have a of creamy coloured swerl in the black drainage. black is good, cream color mixed with the black indicates wet oil.
-Add another 1/2 ml of acid to the mix. remember the heat must be on during seting time AE will not work if you loose the heat. You used, 7 ml of methanol for this batch that should be enough providing you didn't loose too much out the vent pipe. Why not add another 3 ml/ ltr of wvo to this batch just to be sure. 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'll go out in an other hour to see what drains off . I did a pH test on the sample that in the water bath it was 7.5 seems high for an acid treatment,but I haven,t been doing this very long. Do you see a pH drop as the wvo converts?
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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heatbeater
-7.5 that can't be right, it should be 2.5 or less for the ae reaction to work properly.
-if there is any ph increase at the end of the ae treatment it will be minimal, but wetter oil will cause the acid to be slightly diluted and that can cause some change, but I have never seen 7.5, the highest I've seen is about 3.5 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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Tom,like you said 7.5 doesn't seem right . I rechecked it with a meter and some new pH strips I got from Rick and get 6.5 ,which is still bad. I know AE will work ,because I have proof with the sample. I made sure the wvo was blended good before I took the sample,so the sample should represent the batch. I also drew some off at the same time and heated to 220F and didn't get any steam. I was pretty sure I wouldn't have any problems with water. Why such a high pH? Residue left in the tank? or something from methanol? I used HEET for the test ,and buy from a local pump for the batches. I can't see where there would be that much residue to cause any problems.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post



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heatbeater
-how are you checking ph of the mix? are you mixing the test sample the same way you do for titration ei oil mixed into IPA? there is no way to check the ph without dilution, in this case the contaminant, sulfuric acid is leached to the IPA and the reading is from the IPA Are you using 91% IPA, what is the ph of that


" 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 pull a 3 cc. sample from the sample jar to run a titration. You can't do a pH right in the wvo? If you dilute it ,that going throw the reading off.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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heatbeater
-no you can't check the wvo directy using a ph meter any more than you can do T on wvo without mixing it in IPA. The dilution is constant for each method and there for not a problem when it comes to reading the results. If you have been using turmeric for T, then you may not like the time it takes to get result using the ph meter. With the meter you have to wait a few seconds or more after each addition of caustic solution for the reading to stabalize. With turmeric the reading is instant, at least thats what I experianced last week. I still need to do more comparasons between the two latter this week. 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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Originally posted by heatbeater:
HI South,is that what you use for AE?
I have not done AE for 4 or 5 years. My oil rarely titrates above 2 NaOH. When I did do AE it was only to see how it worked and then only a liter at a time. As I recall, I think I got my H2SO4 from the High School Science Lab.

When I was running my tests I did not keep heating the Oil. As long as everything remains liquid the reaction should keep going along at a reduced rate as the oil cools down.
 
Location: Southside | Registered: January 12, 2010Reply With QuoteReport This Post
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SB
-in test we did last spring for the start of the AE thread, we had AE mixed and hot, and another sample mixed hot and allowed to cool 30 days later the cold sample had NO reduction in ffa while the hot(140f) sample was finished in 12 hours. The whole idea behind the cold test was to see if we could mix in the acid and methanol in the 45 gal drum of wvo for later base reaction. 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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A couple of things ,to me happened . I lost methanol thru the vent,but to me it seems impossible to lose enought to kill the reaction. Can methanol go alkaline or lose its effectiveness if it sits? As an experiement I 'll try to got some methanol from somewhere else.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post



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BioTom,
when I did my Acid/Base testing I used the FATTA method. My testing showed that Temperature was only important in so far as the cooler the reaction the longer it took.
One of the other fellows who was using Acid/Base at the time said that he sometimes had to let the reaction run for 2 or 3 days when it was unheated. He did mix it now and then over this time but not constant mixing. Apparently during AE the reactants do not drop out the same way they do when doing the Base transesterfication stage.

I assume you did get an initial drop in titration in your "Cold" batch because it was mixed hot and then allowed to cool. What was it's titration drop after 6 hours?
What did your testing show the critical temperature to be that if the reaction fell below no further reaction occurs.

Did you stir the oil a couple of times a day over this thirty days? Did you do a Titration each day to check what was happening?
 
Location: Southside | Registered: January 12, 2010Reply With QuoteReport This Post
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no you can't check the wvo directy using a ph meter

I did a pH test of the batch again,disolved the wvo 50/50 in IPA ,and got a reading of 3.5. That's alot better. Did a titration this morning and its still at 10, and it was heated and blended good. So, it looks like I'm going to have to redo this batch somehow to get it lower in T. I'm thinking the nights are still going down near or in the 30's which makes it hard to keep temps above 120F. I think heat is important,but don't boil off the methanol.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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