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My second AE failure using recovered methanol
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I just ordered a methanol test kit from Utah biodisel supply. I should have ordered one earlier. I did AE on what I call my 'normal wvo' and its still titrates 12. I used methanol from my 'still'. Usually after AE and letting it sit overnight it'll drop to 4-5. Once I get the test kit I'll find out. First batch contained some liquid fryer shortening and didn't respond that good either.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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Heatbeater
-NEVER use revovered methanol for AE unless you are sure it is 99% methanol, keep it for base process and mix 50/50 with good methanol. The water in the recovered methanol stops the AE process. 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 ,thanks for the advice . Maybe by the end of next week my test kit will come and I can check the purity.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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Anyway ,am I going to be able to another AE to drop titration? and how would I go about it?
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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heatbeater
-the short answer is yes Wink The water in the methanol is most likely the cause of this failure, or a combination of water in the wvo and methanol.
-mix up a normal T sample from the wvo/methanol/acid mix. now calibrate your ph meter and check the ph of the sample, I,m sure it will be ph 2.5 or more (not good), slowly add more acid to the processor and mix, do this in small steps there is NO advantage to adding too much acid, recheck the ph, you need to reduce the ph to 1 if you can, this will result in a good AE.
-also add 2 or 3 ltrs of new methanol to be sure you have enough for the 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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Thanks for the advice Tom. It'll be awhile before I can get some good methanol once I do I'll give it a try.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post



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Originally posted by heatbeater:
I just ordered a methanol test kit from Utah biodisel supply.
All you need is a hydrometer.
They make a special hydrometer called an Alcometer Tralles which is a hydrometer calibrated to read the % of alcohol direct. While it is technically made to measure ethanol, in reality ethanol and Methanol have almost identical SG and it works fine for methanol too.
The last one I bought cost about $7.00 at a home brew shop like this one.

http://www.midwestsupplies.com...alle-hydrometer.html
 
Registered: June 27, 2010Reply With QuoteReport This Post
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3 Options

1)molecular seives

2)more methanol

3)or start over.

To start over you can boil off the bulk of the methanol and then settle out the acid and the water. You can then start over as if nothing ever happened.
 
Location: CO, CA, KS, or FL | Registered: January 17, 2009Reply With QuoteReport This Post
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I just got my hydrometer to check the purity that I've been getting out of my condenser,no wonder the last 2 AE's that I did failed. It's running about 91% purity. Some methanol that I bought a ouple of months ago is running 98.7%.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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It's running about 91% purity

heatbeater
-Norman at Nebraska BioPro has molecular seive that should remove the water from the methanol I haven't tried it yet, but bought 3 bags when I was there this past spring. 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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mix up a normal T sample from the wvo/methanol/acid mix. now calibrate your ph meter and check the ph of the sample, I,m sure it will be ph 2.5 or more (not good), slowly add more acid to the processor and mix, do this in small steps there is NO advantage to adding too much acid, recheck the ph, you need to reduce the ph to 1 if you can, this will result in a good AE.
-also add 2 or 3 ltrs of new methanol to be sure you have enough for the reaction Tom

2 or 3 liters of new methanol should enough for 40 gallons wvo? If I've pulled that much water vapor from my BDG than it seems to me that the methanol should be reduced to a safe level in the BDG for soap making.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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heatbeater
-if you used 16 ltrs of methanol for the AE, then you added 1.44 ltrs of water (9%) to the AE mix, not a good thing for sure. I would add 5 ltrs of good methanol to counteract this, and if you can check the ph of the mix I have never had an AE not work when the starting PH was one (1)
-I am a bit concerned on how much soap will be produced in the base stage with that water content are you base processing with KOH or NaOH? 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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After AE I base process with KOH ,but it never passes 3/27 so after at least a day of settling and draining off the glycerin I do another base process using Naoh,which will pass 3/27. That amount of water does worry me,but I don't know of any way to get rid of it. I do dewater my wvo before doing the AE by heating to 230F and use an air bubbler and pump circulate every couple hours. I don't know if I'd want to heat it that high with methanol in it,unless I take it slow.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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I used 3.5 gallons(13.30 liters) of methanol with 180 cc. of the acid (ROOTO). For a 40 liter batch of wvo I use 3.5 gallons of methanol for AE and 4.5 for the first base reaction,and about 2 gallons for the second base reaction. Tom, what your saying is circulate this batch and add acid until the ph drops to 1 and then add a couple of liters of good methanol? I normally add the acid to the methanol. I've never been able to get AE reactions to work by adding acid and methanol separate. I know you do it that way since you had a close-call. In this case I'll do it separate so I can get the ph down. With 13.3 liters of methanol and 10% water it's about a quart of water to the 40 gallons of wvo. It doesn't seem like much water ,but it did a good job of messy up the last two batches.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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To start over you can boil off the bulk of the methanol and then settle out the acid and the water. You can then start over as if nothing ever happened.

I could do it this way. I think I could boil the water out ,since I can remove the reactor lid,but I don't like the idea of methanol vapors floating around in the small shed I use for bio-brewing unless it's windy out.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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Heatbeater
-You have distilling capabilities so starting over is for sure an option. As far as just boiling the methanol/ water off in a small shed, that seems a bit risky to me.
-As far as how you mix or add the acid: it makes no difference to the AE reaction. If you add acid first, then the biodiesel will be a darker color than if the methanol was added first. If you experienced problems by adding the chemicals separately then something else was causing the problem. I add methanol, mix then add the acid. When you add acid to the methanol, you have to handle all that acidic product, for me that just adds another area where accidents can occur. Ideally, I would like to have a separate AE tank and similar mixing and entry system as the processor tank that would make the premixing and entry of the acid and methanol mix a none issue as far as safety goes.
-Ph 1 (one) is the target ph for me, as I said in the previous post AE has never failed at this level of acidity. How much acid you have to add to this batch is another question, it is something you will need to experiment with. First drain a few ltrs from the bottom of the processor, much acid and water will be there. Then mix well and draw off 1 ltr, from this mix up a normal T sample and check the PH, add 1 ml of sulfuric acid and re check, repeat until the sample reaches the target PH, then calculate how much extra acid to add to the batch. 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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How do I use the meter to test the wvo? Do I dilute it some how? I don't think I can test straight wvo ,though I'm not sure.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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[QUOTE]Then mix well and draw off 1 ltr, from this mix up a normal T sample and check the PH, heatbeater
-yes dilute the wvo mixutre as you would when you are doing Titration, i use 4 ml of wvo in 40 ml IPA then insert the probe and let it sit there for about 5 minutes, it will take that long to stabalize the reading.
"add 1 ml of sulfuric acid and re check" quote
-add 1ml of acid at a time to the 1 ltr of wvo that the T sample was taken from, not to the T sample


" 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 advice in a day or two I'll do some testing and post the results. I which I had more time to do more bio-brewing but right now I got some projects to get out the way before the winter cools down. Maybe a dry wash system would cut some of time out. It's something I'm going to check .
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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