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Wash problems after HTAE High Temp Acid Esterfication
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i forgot to add that I am taking The 150 gallons in my wash tank and misting it for 24 hrs (1hr on 1hr off) at a rate of 1/2 gallon per minute and see what I get.
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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lew
-keep me posted, I started a wash to day, on a 160ltr batch that was not neutralized, so we can compare notes. 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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Lew,
Yours sounds like the classic case of just needing more drying time.
What is your drying method?
I've had several batches over the years that seemed rather stuborn when it came to drying. Classic test being that it clears at elevated temps then clouds again upon cooling.
A soap titration is the most accurate way of determining soap content in the fuel.
Just my .02
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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Double D

I dry by pump and splash with an air stone in the tank to provide more to push the wet air out of the tank. I'll have to do a search on soap testing, never done it before. Just a new learning curve. Problem is, everytime I learn something new, it starts a new project. Just what my wife wants to hear.

Biotom

My sample that I split in half didn't do what I thought it would. Both halves have a quarter of an inch of clear bio on top and the rest is cloudy. This is 12 hours into test. I'll seee what it looks like tonight and let you know. I haven't had a chance to go to the "lab" and see how the 150 gallon batch is doing with the extra washing yet. Got to go to work
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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Biotom

Samples are both now 75% clear, no appreciable difference between the two. But A good difference between The original sample with 1 additional wash and the 2 split samples with an additional additional wash, if that makes sense.

15o gallon batch. 24 hours of 1/2 gallon per minute mist wash 1 hr. on, 1 hr. off, 1hr. on, etc. this larger mist head spits the mist out a little further than the 1 quart mper minute head and was actually beating the surface of the bio pretty harder. It definitely would have made an emulsion if it were a first wash. Any way, I checked at the 24 hour mark and the surface had a scum of froth on top. I suspect this is a soap froth and that is the issue with why it won't dry, it needs more washing even though the wash water was clear. I will let the batch settle over night, drain and try drying again.
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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lew
-I'm not sure if the water quantity plays the same part in causing an emulsion with mist washing as it does for pump washing (thats what I do) this is very vigerous, add a bit too much water and your in trouble. the batch I started to wash today, had suspended byproduct from the repo, I would normally static wash , but decided to try the water quanity theory, added 2% water/volume of bio, and pumped for 5 minutes. after 3/4 hrs, I drained, no sign of an emulsion. I have since repeated 3 washes (15 min) at 5% water and it is looking very good.
-I should note, this batch was not neutralized prior to washing 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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Biottom

I have never done a pump wash. To scared of the risk of emulsion (have those issues with mist washing). However, this batch may warrant a try. The vigorous shaking I did with the 2 samples I have sitting on my counter had no emulsion problems (they shouldn't, they have been washed several times). YOur saying to add 7.5 gallons (5%) water to my 150 gallons bio and pump wash 5 minutes let settle, correct? I have a cone bottom wash tank with a suction line tapped into the tank about 6 above the bottom connected to my pump. I am assuming 7.5 gallons above this pipe because the water below this will not be pumped into the bio. So I could just pump this water back into the tank and recirculate for 5 minutes? It doesn't seem that this would really get the water circulated through the bio enough. For this size batch I think I would have to recirc. for a longer period of time until I got a homogenous mixture. what are your thoughts? BTW My pump is just a little harbor freight pump, not much volume for this size tank.
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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Biotom

Forgot to mention that the 2 samples on the counter are now crystal clear with just a very thin layer of haze between the water (clear) and the clear bio. Maybe 1/16 inch.
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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Biotom

150 gallon batch still settling. I don't know how far in the tank the soap has settled to. It is crystal clear on top, but my upper drain on my wash tank (about 5 gallons above bottom of cone bottom) still shows cloudiness. Time and patience I guess.
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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lew
-Is the bio sitting on water? The last batch I washed 6 times, 5% water each time, it worked very well, I'll take pics of the samples, seems that the wash was finished after the fourth, that batch was not neutralised prior to washing and the differance was like nite and day. 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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Biotom

No, it is not sitting on water. Do you think that would help and if so why?
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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biotom

bottom layer in wash tank STILL cloudy, top clear. took sample off bottom of tank and placed air stone in it over night. If soap was making the bio cloudy then all the agitation in the world wouldn't clear the bio , right? next morning, the sample was crystal clear. So I took turned on my pump to recirculate and splash dry. 24 hrs later still cloudy. This is getting frustrating.
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post



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Lew,
Are you heating your bio before or while spray drying?
Heating your bio dramatically accelerates the drying process.
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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lew
-frustrating, probably an understaement Big Grin washed biodiesel will clear completely even while it sits on water. methanol or soap will hold water in suspension and cause the turbidity that we have. The question I have is why is this batch so difficult to wash. could be but not likely underreacted, or reacted and washed at too high a temp which will cause monos to be created. monos will really affect the wash process, wether they are from unreacted wvo or reverse reaction. the problem there is we can only speculate since we can't check for them without the fancy equipment. 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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Double D

No heat. I have always done a cold wash. The only problems I have ever had are emulsions. Fromwhat I am reading I think I may have a Monoglyceride problem.

Biotom

I think you may be right about the Mono's. I always try to base process at 140F. Maybe i producing Mono's and that is why I am having not only difficulty washing this batch, but why I have always had emulsion problems. I have 1 more 150 gallon batch to wash after the mess I am in right now. Then I will start base processing at 120F instead and see if that changes my wash problems.
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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