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Wash problems after HTAE High Temp Acid Esterfication
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This last batch is the worst, two complete wash and dry cycles and no cigar Mad the bio will not clear. I'm wondering if the high temp in that process is setting the stage for a reverse reacion which would create an abundance of mono and diglycerides. I should note that this was high conversion bio, 6/27. or could it be that the base reaction was pushed too far, and the only chemical reaction left for the added methoxide was reverse
-I read a post today by RickDaTech that says mono's and di's are hygroscopic, and can cause this type of result.
-all is not lost, the bioler seems to like the stuff, yeas , heating season has started!
-I'm washing another batch to day, and so far it doesn't look good! 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, the HT has nothing to do with the base stage unless you are processing at HT also. At normal temps, the base stage 3/27 test is either converted or its not.
Take a sample, heat it, and do a small test batch and see if any more gly drops out. Otherwise I would say that there is soaps keeping the bio from drying. Im washing a btach right now that passed 9/27 and it was soapier than all get out. small emulsion, 4 washes still cloudy etc. I thinks its from pushing the reaction so far. 2 reprocesses after a 3/27 pass on the single base stage
 
Registered: May 13, 2008Reply With QuoteReport This Post
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hook
-pushing the reaction too far can result in more soaps, accoring to the reply I just recieved from my chimist friend, Jim. he says this is caused be reverse reaction, creation of mono and biy's, he also said not to worry, because they will wash out, that is news to me, but since I don't have the testing equipment,(he does) I can't confirm this.
-the batch produced much more foam when it was drained into pails, which to me would indicate soap. That being said, no soap will wash out, as I said the wash water is clear. that leads to the next possability, the water used for the wash is well water, that has a very high iron content,and god knows what else, to the point, sometimes the water is slightly black. I have to run the well pump for 30 min before adding water to the wash tank. The part of the water that attracts the soap, ion, seems according to Jim that the iron will fill this space and then the soap will not have any attraction. have you ever heard anthing like this before.
-I am starting a new wash today and will use hot soft water from the house to see if that makes any differance. 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, Im also on a well with high iron. My lines to the barn run off the soft water. What I can tell you is that I have noticed that if I start washing on hard water when I run out of salt, finish on hard water(clear wash water), refill the brine tank, wash once more on soft water, the water comes out cloudy again. I dont know if that makes sense. You can think of it this way...hard water has a lot of dissolved particles. Those particles take up space in the water that otherwise would be occupied by soap. So soft water has less disolved particles, and can fill up with more soaps before it reaches the point of saturation. Hard water saturates quicker than soft water.
Hope this helps you out, let us know what happens
 
Registered: May 13, 2008Reply With QuoteReport This Post
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Hook
-you just confirmed what the chemist, Jim told me. I will find the email, it explains why iron laden water can be problimatic. thanks for your response. Seems, and now I would bet on it , the problem has nothing to do with htae, and everything to do with water quatity (buckeye you can breath easy now). Didn't have that problem all summer, when cattle where grazing, but now that there gone the well just sits and stinks Big Grin 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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didnt know you ran cattle Tom, what breed(s)
 
Registered: May 13, 2008Reply With QuoteReport This Post



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Hook
-how much water do you use for one wash? I just tried the method recommended by Jim, I used 10% (he recommended 7, I don't follow instructions very well Big Grin) water, heated the bio to 55%max, then added hot water 16 ltrs drew down a vaccuum of .5 bar about 14.5" Hg. and pump washed for a full 15 minutes. separation within 10 minutes, and it is supposed to be ready for draining and a second wash in 45minute. man that is fast. 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 bubble wash and add 15 gallons water to 50 gallons fuel. so about 30%
I bubble wash after one static and run longer bubbling times, 8-10 hrs each wash. Usually 3 washes plus static gets it done.
 
Registered: May 13, 2008Reply With QuoteReport This Post
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I am nnow having the same problem, the bio won't dry. I mist washed 150 gallons at the rate of .25 gallons per hour for one hour, let it settle an hour, mist an hour, settle an hour, etc. for 24 hours. My cone bottom wash tank lets me accumulate about 15 gallons of water in the bottom before it is pushed out the overflow. I drained the water in the bottom of the wash tank and it was almost crystal clear. So I misted in another 15 gallons of water then added an air stone hooked to an aquarium pump and bubble washed for 24 hours straight. Drained water at bottom and water was clear. I thought it was time to dry. I turned on the recirculation pump to splash dry and 12 hours later the bio still is murky, just like when I started. I do all of my washing and drying at whatever temperature the shed is, right now it is holding in the mid 50's to 60F range. Any thoughts?
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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I also brought a sample up to the house to let it set in a warmer environment overnight at 70F. Usually this will dry and be bright and clear by morning. This sample has only a quarter of an inch on the top that is clear. The rest is very murky. Maybe more washing?
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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lew
-are you washing hot or cold, hard or soft water? 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

I am washing with cold water. Whether it is soft or hard I don't know as our water softener is on the fritz. I do know that when the softener was definitely not working that i could get the bio to wash, albeit with difficulties at times but I worked through them. I took the sample that I had brought up to the house to a constant 70F overnight and put it in the microwave to warm up it up. I got it as hot as a cup of coffee and it went nice and clear with a little bit of white sediment on the bottom after settling about 15 minutes after heating. I thought great all I have to do is heat it up. BUT, I just came in the house for lunch and the sample is all murky again and the house temp. is still 70F. This batch was made with PHO but that shouldn't cloud at 70F should it? If so, I've got a major problem because I have over 700 gallons of this stuff to process and I don't like the idea of heating my fuel tank. By the way, I use this for my heating fuel, but I want to make it meet specs before I decide to run it in my truck. Furnace parts are much cheaper.
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post



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lew
-cold water washing takes many more washes to get the soap out (I always washed with cold water until a few weels ago) Warm water is a much better way to go, the ions in the water are really moving at 50C and that helps to recover more soap. The problem I had with hard water was the water from the wash would come crystal clear, but the bio would be cloudy. It seem the iron in the water causes this, it is attracted to the ions, leaving no room for the soaps.
-I also notice that after htae, base, base, neutralize. then wash, the salts created are then disolved in the water, I wonder if this is causing the bio to stay cloudy? I have just completed the seventh wash, using 10% water by volume of oil, and the bio is still cloudy, and once dried stays clear at room temp. This bio should clear sitting on top of the water if the contaminants are removed. I like you, need more washing Big Grin Prior to htae did you have this problem? I have to wonder about the high temp, is it in some way setting the batch up for reverse reaction, which would create more mono and di glycerides, these can cause washing problems. My next batch will be at a lower temp, just so I can compare. 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

Prior to htae I didn't have this problem, but I had an consistent emulsion problem.

If what you are saying is true, that I need more washing, would I still have crystal clear water after a wash that wasn't the last one? If that makes sense.
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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lew
-unfortunately, if you have water with a hight iron count, the the water will be very clear, but the bio will still have soap. Take a sample jar and 1/2 fill with this problem bio, shake the chit out of it and observe, if the head looks like the head on a good beer, you have too much soap. In the past, have you ever let the finished bio stand in a 20ltr pail for a few days, was there any brownish red residue settled at the bottom? I have seen this from time to time, and this seems to be an indication that the water has too much iron. I will post pictures later this evening.
-the consistant emultion problem can be related to byproduct in the wash, monogycerides from underreacted wvo or reverse reaction, using too much water, washing with cold water, to name the most common causes that I know of 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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this photo shows the residue wiped from the bottom of a pail no doubt that this is rust that was held in suspension in the biodiesel and settled over a period of one week!





-In these photo's,the pop bottle on the right was from the previous batch and was washed with hard water. Note how clear the water is, no soap what so ever! after two complete wash and dry processes, the bio was still not clear and I sent the whole batch to the bioler.
-the small jars are from the batch that is being dried today! Note there are samples from 5 washes, prior to these, the bio was static washed X2 with the cold hard water. then washed 6 times with soft water, there is no sample from the first soft water wash. it may be a bit hard to see, on the first sample there is NO indication that the wash picked up any soap, the first wash was the same. the remaning samples have a thin soap layer. This wash was really affected by the hard water in the prewash, and even after 6 pump washes, the rust was still in suspension. Tom

This message has been edited. Last edited by: Biotom,


" 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

So how are you handling this? Just keep washing. In the past I have had no problem with gettting the soap out. When the water ran clear, start drying. Are you saying that the HTAE is making the soap somehow different and must be washed differently? The last wash I did was on AE oil but it washed easily with about 10 gallons of emulsion layer for a 150 gallon wash batch. NO emulsion on this HTAE treated oil, but the soap won't leave.
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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Lew
-I’m not sure what the answer is at this point Confused, I will keep plugging away, and see what happens. I just sent yesterdays batch, the one in the sample jars off to the boiler Mad. This batch was 100% better than the previous one, but the final product was not as clear and shiny as I like.
-Today I start a wash on batch # 3, this wvo has not seen the hard water from the shop so it will be interesting to see how it works.
-I spoke (email) with the chemist about the possible detrimental effects of htae, he says no way! The only effect would be that the process would react faster!!!. So that is good news. His main concern is the water quality and quantity. Any reverse reaction, and he doubts this could even happen in htae, would be corrected in the subsequent base stage.
-I am wondering out loud, if neutralizing the whole batch has a cause factor here, This and htae are the only changes I have made to my process, so one of these, or a combination, is responsible I hope! I’ll keep you posted on this wash, and I am also starting an ae treatment tomorrow at low temp, 130F under vacuum, to see if the vacuum will speed the process without the additional heat. 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 Biotom:
-I am wondering out loud, if neutralizing the whole batch has a cause factor here, Tom


I think you may have found the most likely cause.
 
Location: central virginia | Registered: March 13, 2008Reply With QuoteReport This Post
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Biotom

-I don't think the neutralizing the entire batch is the problem, because I do not neutralize my batch before sending to the settling tank and I am having the same problem you are.

-The other night I brought a sample of the cloudy bio to the house to see if 70F heat would do anything. It didn't help, so i put it in the microwave and warmed it up fairly hot. Went instantly clear. Huh! Let it sit overnight uncovered and it was cloudy in the morning again. Huh!!. So this same sample sat on the counter 2 more days uncovered and voila it was clear!! What happened? I took the sample and shook the crap out of it and it stayed clear. So I took the sample and split it in half. One half still in the original container added water and shook the crap out of it and left it to settle overnight with no cover to see if there was soap that had settle to the bottom and if I could recreate the cloudy bio that won't dry. The other half I took and added water, shook it up and will dry it and see if there is any difference between the two samples.
 
Location: smithville flats, ny | Registered: August 28, 2008Reply With QuoteReport This Post
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