Biopowered - vegetable oil and biodiesel forum
Biodiesel => Chemistry and process => Topic started by: zatawitono on October 06, 2014, 04:08:24 PM
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hello guys , this is my first batch
first , i heat up wvo untill 47celcius .
then i mix methoxide that contain 4 liter and 350 gram naoh
after that i put more 12 liter methanol .
mixing around 1.1/2 hour .
then let it separate around 1 hours .
then who knows 1 batch of it become jelly .
question : what cause it become jelly ?
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Almost certainly water, either in the oil, or because the methanol isn't pure.
How are you removing the water from your oil before processing? Did you do a hot pan test?
http://www.biopowered.co.uk/wiki/Hot_pan_test
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Some jellies can be cracked by adding *more* catalyst and meth, however, certainly not all - so do a test.
If you just add more to the wrong type, it will go from jelly to hard lump.
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this is my jelly batch after do that process . please give me advise .
thanks a lot .
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What was the feedstock?
Photos look like you have liquid on the top and something quite substantial below.
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The feed stock is wvo. actually that is no liqiud on the top. later i use my hand to stir it. Later i founded that has a liqiud that already mixed up with jelly and the liqiud feels very cool like methanol
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You don't want to be sticking your hand it!!!!
Methanol can be absorbed through the skin ... believe me I know!
Was it all liquid oil with no whites? You need to get the oil to at least 80 - 85°C and run a venturi and condenser or pump it in a gentle spray (lots of ideas on the wiki) to get it really dry.
As has been said above try reprocessing a small sample.
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That looks like what I made with creamy oil from a Chinese restaurant during my first year of biodiesel brewing. Resembled turds and was totally unpumpable. The only batch in years of biodiesel making I didn't manage to recover.
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Thanks for your advise.
So the problem here is. the wvo has alot water?
No white mean? Sorry i dont get it
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That looks like what I made with creamy oil from a Chinese restaurant during my first year of biodiesel brewing. Resembled turds and was totally unpumpable. The only batch in years of biodiesel making I didn't manage to recover.
So how you set those creamy oil? can make it into biodiesel?
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By "whites" people mean nasty creamy oil. The only way is to boil the water out (it stinks!). I heat my oil to over 100C, but you can do it at a lower temperature with a diffuser - see:
http://www.biopowered.co.uk/wiki/Diffuser
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can i ask now ?
how to clean up this tank ?
thanks all .:)
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Did you get glycerol out before it turned to jelly?
If so...
Take a small amount (1 ltr etc) and add 150ml more methanol, with 3g of caustic added to it (mix the methanol and caustic before additing them to the 1 ltr)
Heat to about 60c, and shake or stir the mixture quite a bit. Then leave it to stand / cool back to the same temperature as the rest. Dont keep prodding it, just let it be.
See if the result is a harder jelly, or a 'cure'.
There is no solution without some tests / experiments as not all batches work the same. You need to test, and find a solution that works - people can tell you the tests, but not what the final conclusion will be : (
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can i ask now ?
how to clean up this tank ?
thanks all .:)
climb in with a trowel and dig it out, messy business this game..
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can i ask now ?
how to clean up this tank ?
thanks all .:)
climb in with a trowel and dig it out, messy business this game..
im not sure , that is the solution .
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that was slightly tongue in cheek, but then i have had to climb in a tank and shovel out gunk myself before.....
is it liquid enough for you pump to circulate it?
have you done a 10/90 test on whats in there?
can you scoop some out in a jug and take a pic?
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Did you get glycerol out before it turned to jelly?
If so...
Take a small amount (1 ltr etc) and add 150ml more methanol, with 3g of caustic added to it (mix the methanol and caustic before additing them to the 1 ltr)
Heat to about 60c, and shake or stir the mixture quite a bit. Then leave it to stand / cool back to the same temperature as the rest. Dont keep prodding it, just let it be.
See if the result is a harder jelly, or a 'cure'.
There is no solution without some tests / experiments as not all batches work the same. You need to test, and find a solution that works - people can tell you the tests, but not what the final conclusion will be : (
I dont get glycerol :(
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If you haven't made glycerol, then you haven't made any bio.
Sounds like water, catalyst and oil have just made soap.
Try the test julianf suggests and see what happens. You should make bio, but with a lot of soap still in the mix.
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If you haven't made glycerol, then you haven't made any bio.
Sounds like water, catalyst and oil have just made soap.
Try the test julianf suggests and see what happens. You should make bio, but with a lot of soap still in the mix.
Ok sir, heat the mixture of methoxide and oil or the oil only?
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NO, ONLY heat the oil (or oil/soap in this case) but be careful, it will contain methanol so don't breath the fumes and don't heat it with an open flame! In fact keep the temperature a little lower than suggested. 40°C should be enough for the reaction to take place. The lower temperature will reduce, but NOT stop fumes being given off so still take care not to breath them in.
Mix the catalyst with the methanol at AMBIENT temperature until it's dissolved, then carefully add it to the oil and mix, again being careful to keep away from any fumes that might be given off. After mixing, leave to stand and see if any glycerol is dropping out.
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Anyway, i already done 5/45 test
The result is around 2ml drop down.
And the rest methanol become yellow colour.
Is that cause by water?
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Bio (the methylesters) is generally yellow in colour.
When you do the 5/45 the methylesters dissolve in the methanol, so that's what colours it.
The test hints at some conversion, so you may be lucky, and the test suggested may push the reaction further on, and then all the glycerol drops out. That's what youre hoping for.
Do as i suggested before, with the modifications suggested by the other Julian, and report back what you find.
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Bio (the methylesters) is generally yellow in colour.
When you do the 5/45 the methylesters dissolve in the methanol, so that's what colours it.
The test hints at some conversion, so you may be lucky, and the test suggested may push the reaction further on, and then all the glycerol drops out. That's what youre hoping for.
Do as i suggested before, with the modifications suggested by the other Julian, and report back what you find.
i already test what are you suggest . the result is the oil become jelly .
i have attach photos . you can take a look
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the other picture
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here
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That doesn't look good I have to admit.
Did you titrate the oil before processing? If so what figure did you get?
Please confirm the pictures are the result of adding 3g NaOH to 150ml of methanol and mixing until dissolved then adding to 1 ltr of the oil/soap?
As a last attempt I'd try massively over dosing with catalyst ... try the same experiment again but use 10g NaOH dissolved completely into 150ml methanol. Heat 1 ltr of soap/oil to 40°C and add the methoxide mix to it, shake/mix well and leave to stand.
If you don't get a bio, glycerol split after that, I think you may have to consider abandoning the batch (I can't think of any other fixes).
Might be as well to start again making VERY SURE you dry the oil and do a couple of titrations so you know exactly what the feedstock is like.
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I use 2stage no titration metode.
But i admit it, i had put water inside but its accident
I want to remake, can i ask?
How to clean up this tank?
I use electric heater to heat the oil, when i heat the oil untill 50celcius. If already 50celcius, i put the methoxide. When i put metoxide, i must turn off the heater or keep it ON but keep on 50celcius?
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if i were you i would put this to one side, pour it in to containers and come back to it another day.
start again, fresh oil, follow advice on here (dry your oil, calculate your chems, mix your chems 10/90...)
does that unit of yours have a lid on it when you are processing? dangerous stuff we're using, be careful..
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How did you accidentally get water into the processor and how much? You didn't mention this before! It makes it very difficult for people to help you if you don't tell us all the facts!
I think the no titration method causes more trouble than it's worth for people new to biodiesel.
It may be better to start again with a simple two stage process ... http://www.biopowered.co.uk/wiki/Two_stage_process (http://www.biopowered.co.uk/wiki/Two_stage_process) using titration ... http://www.biopowered.co.uk/wiki/Titration (http://www.biopowered.co.uk/wiki/Titration) and ... http://www.biopowered.co.uk/wiki/Titrating_with_turmeric (http://www.biopowered.co.uk/wiki/Titrating_with_turmeric)
Before giving any further advise I think we need to know more about your processor. That way we can tailor advise to suit your plant. Most of the advise to date has assumed that you have a GL type processor.
Is this your processor ...
(http://www.biopowered.co.uk/forum/index.php?action=dlattach;topic=2189.0;attach=139;image)
As has been mentioned above, does your processor have a lid?
Is the wire in the tank your method of measuring temperature?
Does your processor have a venturi and condenser?
Are you using a pump for mixing?
What method of drying the oil are you using?
It would help if you can post photos of the whole processor.
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sorry before i dont mean it . i just remember . i think its a lot .
my place is hard to find isoprophyl alcohol , so i decide to use 2 stage with no titration
i have attach a picture of my processor .
before i dont drying the wvo . no i already know thats wvo cant contain water for going to process .
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Can you answer some of the questions in my above post please?
At a quick glance, your processor looks rather basic and may need some modifications to make it run safely and efficiently.
What size is the pipe work and what is the pipe work made from?
What size is the pump?
How are you controlling the temperature?
Have you tried looking on EBay for isoprophyl alcohol? There's plenty available on eBay UK but when I look at eBay Indonesia, it refuses to return any search results.
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Is the wire in the tank your method of measuring temperature?
yes , its is . that wire is my thermostat wire .
Does your processor have a venturi and condenser?
i dont using venturi and condenser
Are you using a pump for mixing?
yes , i use pump for mixing
What method of drying the oil are you using?
i dont drying the oil before
At qick glance, your processor looks rather basic and may need some modifications to make it run safely and efficiently.
yes , please tell me which part i must modification
What size is the pipe work and what is the pipe work made from?
my pipe is 1/2inch , made from black steel
the size of my pump , i dont know so well because its information already broke .
i using thermostat to control its temperature
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OK, it's probably not worth trying another batch with what you have there. The pipe work and probably the pump is way too small for the size of the processor.
If you do get a conversion, the most likely thing will be that the glycerin drops out and the pump will only be circulating a small amount of glycerin rather than mixing the oil and methoxide. Also with a very small and slow flow the methoxide (being less dense) is likely to rise to the top of the tank and not get mixed in the first place.
To get good mixing, you need pipe work of at least 1 inch preferably bigger. Try and avoid elbows (sharp bends), use radiused bends. Although you don't have the rating plate, I'd guess your pump is way too small too. Big pumps give quick and more complete reactions. Try and find a pump of least 80 litres a minute, preferably much bigger.
Make a pocket for your temperature sensor, so it won't effect the seal of your processor lid. And make sure you have a lid (you still haven't confirmed your processor has one). It looks like a clip top barrel you're using ... get a lid and make sure it's air tight. Having done that, fit a vent ... VERY IMPORTANT. Run the vent pipe to outside away from windows, people and animals etc.
Consider making a venturi and condenser (loads of information on the wiki ... look at the GL style processor page) This is probably the safest and most efficient processor you can make.
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Probably possible to make bio with limited pipework and pump if you stop periodically to drain the glycerol?