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Poorly converted!!
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Has anyone had issues with filtered oil from a restaurant filtering out fit? I believe that this oil is filtered thru Magnosol. It appears to be under converted and there is what appears to be a Plastic waffle on the top. When left to cool the whole batch (1liter test) turns to jello. Any body experience anything of this nature??
 
Registered: March 26, 2016Reply With QuoteReport This Post
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Hi Uncle Gene,
Welcome to the forum.
quote:
Originally posted by UncleGene:
Has anyone had issues with filtered oil from a restaurant filtering out fit? I believe that this oil is filtered thru Magnosol. It appears to be under converted and there is what appears to be a Plastic waffle on the top. When left to cool the whole batch (1liter test) turns to jello. Any body experience anything of this nature??

Yes, I have seen something similar.
I assume you are using NaOH/ Caustic soda/ sodium hydroxide in the reaction.
The things that causes the thin film on top is soap settling out on top as methanol evaporates.

Things that might cause the whole batch to turn to jello includes but is not limited to:
Water in the oil
High titration oil
Too Much NaOH used in the reaction
Not enough NaOH used in the reaction
Not enough Methanol used in the reaction
Wrong tune playing on the radio

Please tell us the following using metric measure when appropriate:
Titration of the oil
Whether you checked for water in the oil
How much NaOH used per litre of WVO
How much Methanol used per litre of WVO
How did you mix your one litre batch
Did you have separation- that means that a layer of "glycerine" settled to the bottom of the container.
Anything else you might thhink is relevant.






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post
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The original batch from the same source was tested a "T" of less than 4 NaOH, heat settled in a Bio Pro 190 and then stirred heat dry to less than 400ppm H2O Sandy breay calcium hydride tester. This batch resulted in non converted, recovery converted and ultimately 70 gal of jello. Note had mixed with some other oil and had complete conversion issues. Another note this oil appears to look like finished fuel in the starting state. Zero H2O settle Heat.
Testing started:
* 1liter oil
* 200ml of CH3OH (20%)
* 6grams + 4 grams for titration. 6 instead of 5.5 have had no issues with other oils
* Oil was heated to 130deg F (Microwave)
* Oil was stirred with Immersion blender Not quite as good as ultrasonic but good 10:00 min until reaction looked complete
* settled and had gly drop. Note previous test had produced a drop as it cooled over nite turned to jello
* Was suggested by Chemist at Spring Board BioDiesel to separate the gly before cooling. This was done on the third test batch,
* this produced a clear sunflower colored oil, 3/27 test was done and produced result of 89-99% (Not acceptable)
* resulting oil was heated and there were bubbles as in a soda did not float, stationary in liquid, not there before re heat. First time to see this!!
* recovery conversion was done with based on the amounts per 50gal (scaled)750g Koh and 2gal as per Spring boards Manual for recovery (500g NaOH)/2gal CH3OH). IE 3.78 grams NaOH/60Ml CH3OH
* Stirred
* Settled had more "dirty"looking gly on bottom as expected. relatively clear on top. After some time the saran wrap film appeared as in all batches as cooled the plastic waffle was on the top and as before the entire batch turned to jello.
As an engineer (not chemical) i would like to get to the cause!
I have a thousand questions that have been put to some of the Industry "Experts" and as yet have not found an answer. Have even explored "gas chromatography" and have been meet with what are you looking for?, If I knew I would not be talking to you. LOL
Also as this oil is from a "Re fry" filtering outfit I think that they are using Magnosol in the industry for filtration. Magnosol is listed as a Coagulant.. Curious.
Have talked to Sac Rendering and their method of producing "Yellow Grease" basic heat settle 200deg F and serious filter, no chemical testing that I Know of. PS this oil has the clarity of near virgin oil. If i have to heat to 200d will need another heating container as the Bio Pro 190 that i am using is set to just below the vapor temp of CH3OH approx 140deg F. Can send pix if you think will help.
Any Ideas???
 
Registered: March 26, 2016Reply With QuoteReport This Post
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Hi uncle Gene,

quote:
Originally posted by UncleGene:
The original batch from the same source was tested a "T" of less than 4 NaOH, heat settled in a Bio Pro 190 and then stirred heat dry to less than 400ppm H2O Sandy breay calcium hydride tester. This batch resulted in non converted, recovery converted and ultimately 70 gal of jello. Note had mixed with some other oil and had complete conversion issues. Another note this oil appears to look like finished fuel in the starting state. Zero H2O settle Heat.
Testing started:
* 1liter oil
* 200ml of CH3OH (20%)
* 6grams + 4 grams for titration. 6 instead of 5.5 have had no issues with other oils
* Oil was heated to 130deg F (Microwave)
* Oil was stirred with Immersion blender Not quite as good as ultrasonic but good 10:00 min until reaction looked complete
* settled and had gly drop. Note previous test had produced a drop as it cooled over nite turned to jello
* Was suggested by Chemist at Spring Board BioDiesel to separate the gly before cooling. This was done on the third test batch,
* this produced a clear sunflower colored oil, 3/27 test was done and produced result of 89-99% (Not acceptable)
* resulting oil was heated and there were bubbles as in a soda did not float, stationary in liquid, not there before re heat. First time to see this!!
* recovery conversion was done with based on the amounts per 50gal (scaled)750g Koh and 2gal as per Spring boards Manual for recovery (500g NaOH)/2gal CH3OH). IE 3.78 grams NaOH/60Ml CH3OH
* Stirred
* Settled had more "dirty"looking gly on bottom as expected. relatively clear on top. After some time the saran wrap film appeared as in all batches as cooled the plastic waffle was on the top and as before the entire batch turned to jello.
As an engineer (not chemical) i would like to get to the cause!
I have a thousand questions that have been put to some of the Industry "Experts" and as yet have not found an answer. Have even explored "gas chromatography" and have been meet with what are you looking for?, If I knew I would not be talking to you. LOL
Also as this oil is from a "Re fry" filtering outfit I think that they are using Magnosol in the industry for filtration. Magnosol is listed as a Coagulant.. Curious.
Have talked to Sac Rendering and their method of producing "Yellow Grease" basic heat settle 200deg F and serious filter, no chemical testing that I Know of. PS this oil has the clarity of near virgin oil. If i have to heat to 200d will need another heating container as the Bio Pro 190 that i am using is set to just below the vapor temp of CH3OH approx 140deg F. Can send pix if you think will help.
Any Ideas???
I am struggling to understand what you did and in which order.
It has been a long time since I did all my experimentation with NaOH.
Let's see if I have deciphered this.

You did a 1 litre test batch on oil that you think titrated around 4 NaOH but you did not actually titrate it??
You used 10g NaOH mixed into 200ml MeOH, heated to 130F and only mixed for 10 minutes because you thought the "reaction looked complete"
There was separation.

"Spring boards Manual for recovery (500g NaOH)/2gal CH3OH)"!
Really!!
Does Springboard really mix metrics measure with US imperial measure in their instruction manual? Unbelievable!

"IE 3.78 grams NaOH/60Ml CH3OH"
I am assuming this is what you used to try to reprocess your litre of "biodiesel"- 3.78 grams NaOH/60Ml CH3OH
In my experience this is WAY TOO MUCH NaOH to reprocess a litre of biodiesel that was made with the expectation it would give high conversion biodiesel in a single stage reaction.
Invariable that much NaOH would result in a gel forming.
Back in the "good old days" the reprocess recommendation was 1g NaOH mixed into 30ml MeOH per litre of biodiesel being reprocessed if the biodiesel was not washed and dried and 1g NaOH mixed into 50ml MeOH if the biodiesel had been washed and dried.

In my experience, once you get to around the 10g NaOH per litre of WVO there is a greater likelyhood of making a gel- Soap.
Amazingly, if you do not move the container the biodiesel is in, it may not look like there is gel, especially in a reprocess. It looks like biodiesel- until you move the container and then you see it is a gel.

The saran wrap film is soap that has settled out as the methanol in the biodiesel evaporates.
You can NOT determine the quality of the biodiesel by visual inspection.

NaOH will keep you "honest"
With the almost complete shift to using KOH instead of NaOH, most of the people making biodiesel now do not remember the good old days when one of the major questions on this forum was about why a gel had formed. Wink

The Gel is caused by soap.
If it were me I would do another 1 litre test batch using fresh WVO that had never been involved in a reaction. I would make sure it was dry, heat to 130F and perform a titration
I would then make my methoide using the formula 5g+ titration NaOH mixed into 200ml MeOH.
I would mix the reaction for a minimum of 1 hour.

Then keep the top on the reactor container closed and see what happens






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post
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Guess i got caught up in the blade of grass.
three different batches were made all three failed. also one 50gal batch was made and was the reason for the 1LIter batches. All batches including the 50g which didn't covert failed to convert to my standards, and thus 1liter batches.
Yes Spring board recommends 500g NaOH and 2Gal CH3OH / 50gal batch for recon. 50gal=189.270589liter
500g/189.27lite=2.641g NaOH and one liter of CH3OH based on Spring Boards Cook book recovery.

And FYI the reaction time for basic 50gal batch is approx 00:15:00 appx and if you look you can see the conversion from the muddy mix to a clearer consistency. The 2hour given in the Bio Pro 190 is way over kill as confirmed by chemist at Spring Board,NOrm at Chandler BioPro, Gradon at Utah Bio diesel Small liter batches (test) are usually done in a 2liter pop bottle and hand shaken. The immersion blender is far more efficient, not quit ultrasonic, but significantly cheaper.
This is the only source of oil that I have had this issue!! I am looking to find some one that has maybe experienced This anomaly.
The methods I have used have been successful with all my other sources.
the non testing of H2O on this batch (guess maybe) a pho pah on my part, All Sources are heat sttled for 24h and if present H20drained and then heate-stir with air flow for 24 hrs. this should bring the H2O down to near less than 1500ppm. ALL other oils have resulted in under 400ppm with this procedure!
Did I mention the oil comes from a RE-FRY (Filtering) I think they are using Magnosol as filtering media, clupert?? Don't Know that is why i am searching.
 
Registered: March 26, 2016Reply With QuoteReport This Post
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Hi UncleGene
quote:
Originally posted by UncleGene:
Guess i got caught up in the blade of grass.
I have no idea what you mean here??



quote:
three different batches were made all three failed. also one 50gal batch was made and was the reason for the 1LIter batches. All batches including the 50g which didn't covert failed to convert to my standards, and thus 1liter batches.
I am still not sure what happened here.
Do you mean that you made one 50 gal batch of biodiesel that did not separate, or it had separation but did not pass the 3/27 test to your standard?
Then you did three reprocesses which all turned to gel?



quote:
Yes Spring board recommends 500g NaOH and 2Gal CH3OH / 50gal batch for recon.
Unbelievable


quote:
50gal=189.270589liter
500g/189.27lite=2.641g NaOH and one liter of CH3OH based on Spring Boards Cook book recovery.
2.641g NaOH is a bit less that the 3.78 grams mentioned in your first post.
Still, it has been my experience that if you use this lesser amount of NaOH to reprocess a litre of biodiesel that was made to a formula that should have passed the 3/27 test in a single stage you will still make a gel.
In my experience this is too much NaOH.
I would start with 1g NaOH mixed into 30ml MeOH per litre of biodiesel being reprocessed and see what happens.



quote:
And FYI the reaction time for basic 50gal batch is approx 00:15:00 appx
There are many variables that determine how long it takes a reaction to go to completion.
These include but are not limited to:
Temperature of the reaction
Mixing vigor
amount of chemicals used in the reaction

Many people have reported having to mix for several hours to pass the 3/27 test using the tiny cheap Chinese water pumps that are so popular.
Myke from South Australian Farmers Fuel once posted to this forum that their commercial biodiesel reactor achieved 99% conversion in 10 seconds.
If you have actually performed testing that shows that your reactor only requires 15 minutes at 130f to achieve completion then that is fine.
Many reactors require considerably more time.



quote:
and if you look you can see the conversion from the muddy mix to a clearer consistency.
I assure you that you can NOT visually determine the quality/ completion of the biodiesel produced.

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






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post



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The only time I made green gel was in the beginning and that was due to not having decent scales. The scale showed the amount I wanted but the reality was that the weight was actually considerably higher, so maybe the scale needs calibration ?



** Biodiesel Glycerine Soap - The Guide
- on 5 continents helping people make & sell soap from the Biodiesel Glycerine.


 
Location: :-) Great White North eh ? | Registered: December 10, 2004Reply With QuoteReport This Post
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I thank you for the inputs but do believe that you are totally missing the mark.
Processing methods have worked for years and CURRENTLY working on different oil sources.
With that being said the anomalies point to some contaminants in the oil i have not yet been able to test for.
Was hoping that someone experienced this and could offer offer an incite to what and how to test for it.
will continue to explore the chemical testing labs
 
Registered: March 26, 2016Reply With QuoteReport This Post
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Hi UncleGene,

As you have a Sandy Brae and have tested the water as being low in the oil (should be <500ppm for best reactions) and you have also titrated the oil, I don't know why you are getting bad reactions usually associated with soap formation.

I have never personally processed oil that has been magnesol treated, although I have used magnesol in the polishing process for biodiesel, I cannot think that some magnesol left in the oil would be a problem to transesterification.
 
Location: YORK UK | Registered: April 27, 2014Reply With QuoteReport This Post
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Hi uncle Gene,

The most likely causes of your problem with the 1 litre test batches are:
1. Reacting for only 10 minutes. Unless you have a very violent mixer this is unlikely to be enough time.
2. Open top container for mixing that allows MeOH to evaporate.
3. Using way too much NaOH in the reprocess (3.78 grams NaOH/60Ml CH3OH).
4. High titration WVO






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post
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thax but i think if you do the math you will find that the nos are close, for both the initial reaction based on Spring Boards, Utah Bio Diesel numbers as well as a host of others and the scaled numbers for recovery. PS this has worked for years with other oil sources. I did that in one of my previous posts. #1 Immersion blender next best thing to ultrasonic. #2 The boiling point of CH3OH (Standard day is approx 64.7degC or 148.5degF) and my reaction temp is near 140degF as optimized from input from above mentioned sources. evaporation time is in the days++ that is why you can't just leave the lid off your Glycerol tho mentholate it. Besides the reaction is CH3OH rich to insure the reaction! And will have to be boiled/vacuumed off to meet the ASTM CH3OH (for flash point Suppression of BioDiesel)
As I said I am looking for some one who has experienced this phenomena and has SOLVED it!!!
All these methods and calcs have worked with all but this oil source!!
As i don't know what the chemical is that is responsible for this reaction I hate to throw $$ at blind testing MIU, Iodine, Yada Yada, I would like to find a test such as "T" or H2O that I could do in the field before pick up. Prior to wasting 50+gal and 10gal CH3OH and respective NaOH or KOH
 
Registered: March 26, 2016Reply With QuoteReport This Post
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Hi UncleGene,

quote:
Originally posted by UncleGene:
thax but i think if you do the math you will find that the nos are close, for both the initial reaction based on Spring Boards, Utah Bio Diesel numbers as well as a host of others and the scaled numbers for recovery.
I have done both the Maths and the actual experimentation.
If your initial 6grams + 4 grams for titration did not give you the 3/27 results you were after just increase the NaOH amount slightly

If you reprocess a litre of biodiesel that was made to a formula that should have passed the 3/27 test in a single stage reaction but did not, using 3.78 g NaOH per litre for the reprocess is WAY TOO MUCH NaOH and WILL produce a solid gel every time.
I have performed the experiments.



quote:
#2 The boiling point of CH3OH (Standard day is approx 64.7degC or 148.5degF) and my reaction temp is near 140degF as optimized from input from above mentioned sources. evaporation time is in the days++
Wrong. At the temperature and mixing you are using evaporation is NOT in the days++, it is in the minutes++.
Back in "the good old days" when people routinely used 55 gallon open top drums to process their biodiesel in they had problems with methanol evaporating during the reaction.
Just put your nose over the container while the mixer is running and smell the methanol evaporating off. Wink
That is why now days reactors (Including springboards) are designed with a closed top- to prevent evaporation.


quote:
And will have to be boiled/vacuumed off to meet the ASTM CH3OH (for flash point Suppression of BioDiesel)
This is totally irrelevant to the requirements of the reaction.
To achieve high conversion biodiesel in a single stage reaction requires an excess of methanol to be present while the reaction is running.
It is only after the reaction is finished that you can remove the excess methanol.




quote:
As I said I am looking for some one who has experienced this phenomena and has SOLVED it!!!
You are talking to him!!! Wink






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post



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OK What is the chemical that is causing the (plastic) TO FORM???
As I believe I have said numerous times in this post:

These methods Have worked on all oil sources for the last 5 years, logical deduction some thing in the oil. If you are Him then you know, and what is the test short of a shotgun guessing game with multi lab testing.
 
Registered: March 26, 2016Reply With QuoteReport This Post
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PS the reaction that predicated this whole fiasco was done in a 190 (LID ON) and produced copious amounts of floating "plastic". Eliminates that train of thought. The ADD attachment seem to want to open the whole "folder" rather than individual "pix" and is to large. If you want to see visually Send "E" to toyshoppe2@earthlink.net, have had success trans pix on that method.
 
Registered: March 26, 2016Reply With QuoteReport This Post
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Hi unclegene,

quote:
Originally posted by UncleGene:
OK What is the chemical that is causing the (plastic) TO FORM???
What plastic???
This is the first time you have said anything about plastic?
All I have read about is the skin of soap that formed on top of the biodiesel which is what I have said several times.
If you are talking about something other than the "saran wrap" as you call it, please explain exactly what you mean.

It has been my experience that when you use NaOH in the reaction there will likely be lots of "floaties" and crap in the Biodiesel. This is soap.
Water wash the biodiesel and it disappears.



quote:
As I believe I have said numerous times in this post:
These methods Have worked on all oil sources for the last 5 years, logical deduction some thing in the oil.
I am still struggling to understand the problem, you just jump all around with the information in your posts about different reactions and reprocesses in a very confusing manner.

Please explain exactly what you mean in your above post when you said:
"This batch resulted in non converted, recovery converted and ultimately 70 gal of jello."
Was there Separation in the initial reaction?
If there was separation what did the 3/27 test show?

As close as I can figure out from your several different posts, you made a batch of biodiesel that did not quite pass the 3/27 test so you used a HUGE excess of NaOH in the reprocess which made it turn into a soap gel.
That is what happens when you use a HUGE excess of NaOH in the reprocess

If this was not the problem please post exactly what the problem was talking about ONLY ONE batch.
Tell the titration of the oil and amount of chemicals used and the reaction procedure you used including how long you ran the reactor.

I assume that when you reprocess you do remove the glycerine layer that formed from the original reaction before reprocessing.

Once again, it has been my experience that when you hit the "magical" 10g NaOH per litre of WVO mark in a reaction there is much more likelihood of a gel forming.

It has also been my experience that when you use NaOH in the reaction there will likely be lots of "floaties" and crap in the Biodiesel. This is soap.

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






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post
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You might have water in your oil or methanol that has caused your poor conversion. Too much water causes poor conversion percentage or even no reaction.
 
Location: Texas | Registered: April 27, 2011Reply With QuoteReport This Post
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AS I SAID ALL OF THE CHEMICAL AND METHODS WORK ON OTHER OILS. JUST DID ANOTHER SOURCE AND WAS 50GAL 99% CONVERSION 95%YEIKD AND LESS THAN 41PPM SOAP (NaOH/ Reaction) THIS IS NOT A PROCESSING PROBLEM IN THE STANDARD SENSE.

That is why i am reaching out to see if anyone has experienced this specific problem with Recovered (filtered)oil form a "Filter Fry" cleaning out fit.

Th plastic i refer to is what appears to be (Like the stuff you fill cracks in the house) if i knew what it was i would not be asking for help identifying the cluperet

AS I SAID THE ATTACHMENT APPLICATION AT THE BOTTOM TRIES TO ATTACH THE WHOLE CAMERA FILE (IE CAN'T SELECT THE INDIVIDUAL PIX)MAKES THE FILE TO BIG TO TRANSMITT.
You can see the "my words, Plastic/Jello with your own eyes" Send an "E" Mail to me @ toyshoppe2@earthlink.net with Poor Oil in the title.

Just a reiteration of sentence one this post I have at least 7 other sources that don't filter their oil and their oil processes well using the same chemical and methods THE only difference is the oil supply, the test avail to the Bio Community water and "T" don't identify what seems to be a chemical problem. Not one batch Four Batches One 50gal and three test batches Failed. Again will send pix if you want to see
 
Registered: March 26, 2016Reply With QuoteReport This Post
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Hi Unclegene,

You seem to not understand that until you answer the questions I have asked I can not help you.
Please answer my questions.

PS I do not open email attachments.






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post



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UncleGene; I worked in a fish and chips restaurant briefly. We filtered oil with magnesol. I saw it done. Later I used magnesium silicate, the active ingredient in Magnesol, to dry wash crude finished biodiesel. Magnesol is used to adsorb or absorb free fatty acids and glycerine, monoglycerides and diglycerides from used oil, thereby extending the time one batch of oil can be used. It removes the breakdown products that occur at elevated temperatures when vegetable oil is used for frying food. It does not put anything into the oil. It removes types of molecular compnents from the degredation of triglycerides. For example, free fatty acids adhere to the surface of magnesium silicate solid, that does not dissolve in oil, then the powder magnesium silicate is filtered out of the oil, which removes the bad stuff from the oil which sticks to the powder that has been filtered out to leave purified triglycerides (vegetable oil). It still seems to me that your oil is wet. Try a hot pan test on your oil.
 
Location: Texas | Registered: April 27, 2011Reply With QuoteReport This Post
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thanks first user of the Magnosol filtered oily. Methods used to dry feed stock oil were used and have consistently produced H2O less than 400ppm (dry) using Sandy Bray water tester. Remember this is junk that is on the top of the processed oil not where the soap layer would be. Anyway i believe that there is chemical in the oil I have yet to identify. I can't send Individual pix via the add attachment function on this page. If you send me an "E" Mail to toyshoppe2@earthlink.net I can attach pix of the 50gal (plastic/junk) that predicated the other test batches. They too can be viewed if you are interested. When and if I find the culprit (Believed to be chemical) I will share first with those of you who have responded and have taken the time to look at the results of the process
 
Registered: March 26, 2016Reply With QuoteReport This Post
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