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have alot of wvo that titrates at 15
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I did AE on a batch of wvo that titrates 15 got it to drop to 6 and then did my methanol KOH reaction but the wash emulisufied and I threw alot of it out. What can I expect for a percent yield on wvo that titrates high? I had a couple of bum batches doing AE and my wife thinks homebrewing is a waste of money . I,m going to have to get it right ,especially now that I'm laid-off .
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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Hi Heatbeater
Sorry to hear you have been laid off-I do not do AE,so can't help-I am sure others will help you
 
Location: UK | Registered: October 14, 2008Reply With QuoteReport This Post
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Maybe I"ll have to go into selling bio for a living . I don't know if it would be feasible but I do have the experience. I was always thinking of some way to make a living in case my job dried up and this is where I'm at.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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Heat
-sorry to here about the job, I think the bio industry would be a good one to get into, it sucks right now with the low price of petro diesel but that can't contunue. My take on that, big oil is trying to close the bio industry down. we need legislation forcing big oil to blend with biodiesel. that law is just comming into effect here in Manitoba, it was a BIG boost to the bio producer (ya, so far there is only one licenced up and running)
-about your wash and the dreaded emulsion. I have been doing so work on this, and with the help of a biodiesel chemist, have determined we wash with toooo much water. As he says, every thing in chemistry (and I know nothing about it) has to have the right balance to achieve a desired result. After reviewing their wash process, I was surprised to see they only use 5 - 7 % water/ boidiesel in the wash. To me this was insane, so I tried it, 160 ltr of bio and 16 ltr of water,( Big GrinI don't follow instructions very well) the temp was 50C this is important, as the ions move at a much faster speed at that temp and therefore attract more soap. the bottom line here, after 15 minutes of PUMP wash (I was in panic mode here Big Grin) there is a very diffinite seperation after 5 minutes. then let it set,for 45 min, drain, then repeat. I should also mention that iron laden water is very problimatic, seems the ions in the water get saturated with iron, and there is minimal room for soap attraction. Hope this helps. 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 , I found out the hard way and that is to always take a jar sample to see if there's any thing that's settling out,and that's where I threw out alot of bio from one batch. I also took a sample of what is supposed to be washed and dried bio from the bottom of a 250 tote and it was not the same as a sample from the top. The bottom sample was cloudy so I added an equal amount of water and shook the day lights out of it. It looked like milk ,all of it. It took a week before it settled into three layers. 1)bio 2) soap 3) water. I,m going to have to draw off the top in small amounts until I get into some that's cloudy and re-wash.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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Interesting about using 5-7 % water and pump washing? By pump washing you mean you add the full amount of water (the 5-7%) and then pump the the water and bio together? Let's see 50 C is what temp F. Repeat the water and bio pump and settle until you have clear water that settles out? Is this right?
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post



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Heat
-did you check out RickDaTech's new biodiesel drying thread, the pictures of washed biodiesel, are probaly the best I have seen!

-yes that is correct. I used 10% water but on the next batch I will use less. the nice thing about this is you are ready for draining in one hour. 50C is about 130f. from what I was told, it is VERY important not to exceed 55C!
-not nessacarily clear water, but when you can see the bio on top of the water starting to clear up I will post you some pics tomorrow. 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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heat
-one more thought about the emulsion, what temp do you do the base process at. Jim the chemist says never never at any cost process at more than 55C. at 65c you start to set the batch up for some reverse reaction which creates mono and di glyceridids, this can really lead to an emulsion.


" 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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quote:
at 65c you start to set the batch up for some reverse reaction which creates mono and di glyceridids, this can really lead to an emulsion

Tom, I take the blended wvo temp up to 145 F before I inject the methoxide but my set-up can't go any higher, one heating element can't hold the temp any higher than 145 F with 140 liters of wvo. I had to do the base reaction twice ,the first time I couldn't get it to pass 3/27. I can't remember the exact figures but I was wondering if to much KOH would lead to emulisions? Any thoughts? I which I had a before understanding of what takes place under various conditions.
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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I have been doing so work on this, and with the help of a biodiesel chemist, have determined we wash with toooo much water. As he says, every thing in chemistry (and I know nothing about it) has to have the right balance to achieve a desired result. After reviewing their wash process, I was surprised to see they only use 5 - 7 % water/ boidiesel in the wash. To me this was insane, so I tried it, 160 ltr of bio and 16 ltr of water,( Big GrinI don't follow instructions very well) the temp was 50C this is important, as the ions move at a much faster speed at that temp and therefore attract more soap. the bottom line here, after 15 minutes of PUMP wash (I was in panic mode here Big Grin) there is a very diffinite seperation after 5 minutes. then let it set,for 45 min, drain, then repeat. I should also mention that iron laden water is very problimatic, seems the ions in the water get saturated with iron, and there is minimal room for soap attraction. Hope this helps. Tom

Hi Tom
Very interesting results your friend has come up with,and may explain why I have never had emulsion problems(yet),even bubble washing right from the off.My wash tanks were polypropylene 80 Lt tanks (2 side by side)from the hardware store which I would put say 50lts - 60lts of bio in ,then because there was not much room left,(and worrying about the tanks splitting!) I would only add 5 lts-10 lts of water (captured rain water from water butts)and do many of these "smaller" washes,until the water stays clear-at this time the bio will clear as well even with the bubbler still running(something I have always thought is strange-get the same result from a shakem test, if you leave the bio on top of the water-it will go clear over some days,even with the cap still on,and all the water underneath).
I have just acquired a much bigger tank to wash the whole batch as "one",with much more water but maybe my thinking is wrong ,and I should stick around the 10% mark and keep doing many smaller washes,like I used to do with my smaller tanks.
What is very important in all of this, is absolutely no by-product, is involved in the wash cycle at all.
Heatbeater.
I think your excess KOH will give you excess soap which is the emulsifier-and maybe not enough washing to make sure it is all gone.
 
Location: UK | Registered: October 14, 2008Reply With QuoteReport This Post
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taralec
-interesting results. I guess it,s all about the chemistery (should have stayed in school Big Grin). Like I said, I didn't think it was possable. Seems to me that a lot of emulsion problems are being cause by the use of too much water. before you change your batch size to allow for more water, wash 1/2 of the bio amount in the current tank, just use more water and see what happens. and about the byproduct in the wash, you are right, except that without a sufficient amount of water to get the soaps active, there is no problem. 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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quick note on washing:

In general it's better to do multiple, smaller washes than one large wash. It uses less water (or whatever you're washing with, an important consideration when you're washing with expensive solvents in the lab) and you end up with a PURER product, assuming proper mixing.
 
Registered: November 03, 2009Reply With QuoteReport This Post



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kevin,
I might disagree here..

let me explain..
wash 1. not counting the prewash with the glycerin still in the biodiesel.
this is a static wash..the larger the volume here the better..this is where I disagree.
static wash...the BD and 'hot' water just sit..no mixing, no bubbles..put the water in a GO away!
8-12 hrs or more..
wash 2. at this point smaller volumes to tend to work better. so I agree after this point..
also at this point if your in a hurry..run the pump..I do. just don't let the BD/water mix go through the pump..I watch at stop before this happens..ah..a + for a plastic wash tank..Smile

as far a reverse reaction..you adding HOT water..from my understanding this STOP the reaction. yes the base reaction not just the AE reaction..

also hotter water holds more soaps than colder water..

heat beater,
if you ever get an emulsion..I find there are a couple of things that work..
HOT water..if you can 200F water..don't worry about reverse reactions..they aren't going to happen.
also just let things sit..even with water..
lets say you've put 10 gallon of water in..let it sit and drain out 5..repeat until the emulsion is gone..yes this works..I cannot count the number I times I did this when I was learning..long before the 27/3 test..you did use the 27/3 test to verify the base reaction was good enough?

biotiom,
I cannot count the number of base reactions that I've done over 65C..think most in the last year..if they were done in my water heater..YES MOST!! I'd have to put a cooling system to keep the temps below 65C..think 170F..not 150F..yes around 170F the methanol boils out.. help to keep the temps down..the reflux column dumps the methanol back into the reaction.


-dkenny


'84 bluebird school bus, DD8.2L turbo( 4/2011, the bus tranny has died..Frown 8.23.11 bus driven to scrap yard Frown )
2006 Jeep Liberty CRD Smile - the wife's
99 dodge 2500 5.9l 24v..-mine Smile
everything run B100 when its warm enough Smile
 
Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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I'm glad I checked on this discussion because I need to brush up on my washing tactics. Can't do any brewing in the winter but nows the time to see where things went wrong ,so they won't happen again. 1) water temperature of 170F,but no higher. Hotter water can absorb more soap. This is something i never tried ,because my set-up won't go that high . I think that can be corrected. Here's a few questions : 1) My guess is it would be better to pre-heat bio to 160-170F before adding the water ,plus the water has to be up to the same temp range(that's a no brainer). I mist wash on the first wash. Realizing that methanol likes water would also explain the emulsion problems on the first wash. So using the higher temp to vaporize the methanol makes sense. Biotom mentioned something about iron in the water ( I have a well) so it might be better to use rainwater. Big Grin
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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heatbeater
-high iron content in the water is a problem! It leaves less ionic(not sure if this is the right word) space for the soap to be attracted to, at least thats what I was told. Jim the chemist gave stringent conditions for water quality, but for me to meet them I would require a reverse osmosis water filteration system, and I don't see that under the Christmas tree Big Grin. Hot water is best, and to avoid the dreaded white stuff, reduce the water quantity! and do more wash cycles.
-Merry Christmass to all 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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Heatbeater
I use rain water collected in water butts (8 off 55 gallon poly drums)of the shed roof.I find it works really well-better than my tap water,but my tap water does have a lot of chalk in it (very hard water)-Have a great christmas
 
Location: UK | Registered: October 14, 2008Reply With QuoteReport This Post
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Merry Christmas fellow homebrewers!!! My water goes thru a softener but I don't think it does much for the iron problem. The way I see it, the ions are charged particles ,positive and negative with opposites attracting , so there's a limited space, but thats the limit of my knowledge. It looks like rainwater might have better results for washing . Its something I'll have to try this summer. Has anybody done anything to check pH of the bio and how that effects the wash results? Biotom, that's something you should ask the chemist?
 
Location: western new york | Registered: November 19, 2008Reply With QuoteReport This Post
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