Biopowered - vegetable oil and biodiesel forum
Biodiesel => Biodiesel equipment => Topic started by: Mark2256 on February 25, 2018, 08:30:10 PM
-
Hello to Everyone and a special thanks to DGS, Dave for recommending this forum.
I am about to start making my first test batch of Biodesiel this week. I have been researching the process and feel I have a fair understanding of the process and the DANGERS involved.
I will be going round to see a neighbour this week as he works for or owns a waiste oil company so I am hoping to obtain a supply of good used cooking oil.
I also have to consider either building my own reactor or purchasing a used one, and whether to use steel or plastic, direct or indirect heating for the oil. I am looking to product about 170 litres every 2 months but more if needed.
Any advise please buget is very tight.
Kind Regards
Mark
-
Hiya Mark and welcome.
Plastic is best avoided if you can - easiest is an old copper hot water cylinder, depending on how handy you are with plumbing!
That or an old steel drum with tank connectors. The hard part with that is fitting a heating element (of course, usually built into a copper cylinder).
-
Hello Tony
Thank You for the reply, Either way a used 45 gallon Oil drum or a copper hot water tank have thier problems, so I was thinking of using an external heater to heat water circulating in an enclosed system, copper water tanks tend to have the emmersion heater mounted in the top. Steel rusts and stainless steel is out of my price range.
So I am thinking a 45gal oil drum modified for conical base, drums are cheap enough
Kind Regards
Mark
-
Hi Mark
Welcome to the wiki and forum.
If you use a copper water cylinder it's normal to use it up-side-down. That way the heater is in the right place and you have a ready made cone bottom ... not the best cone bottom, but a cone bottom none the less. It's also pre insulated.
Use a short immersion heater so there's less likelihood of the heater becoming exposed should the tank level drop for any reason.
Tony did a good page on copper tanks on the wiki ... http://www.biopowered.co.uk/wiki/Hot_water_cylinders
Neisel (Neil) (another member on here) and myself are possibly looking to buy some chemicals from a chap about 30 miles from you who's packing up bio production. I'll probably be talking to him tomorrow evening and I can ask if he's looking to sell his processor ... Neil advised it was broken, but a repair may be easier than starting from scratch. He also has a large quantity of oil to get rid of ... let me know if you're interested and I'll ask when I phone.
-
Hi Mark, Welcome to Biopowered, nice to see you have made the move from infopop. I've just sent you a pm on there explaining that hardly anyone here in the UK titrates any longer. We mostly use 10/90 dropout tubes and a 2 stage process which is a much more accurate and simpler method than titrating.
Just ask any questions you have on here.
These are the tubes, contact neisel if you want one, Dave.
http://www.biopowered.co.uk/forum/index.php/topic,1504.msg17642.html#msg17642
-
Hello Julian Thank You for the reply I will have see what I can find in the way of a good used copper cylinder thier are some on Ebay but are to far away from Eastbourne. So an ad on Eastbourne, Bexhill, Lewis and Brighton Freegle may produce something.
Hi Dave I will have to waite a couple of weeks to get the 10/90 tube as I have just had to payout for a part for my wifes mobility scooter. So I will try 1 batch useing Titration. I do have 2 small batches of used cooking oil saved from home 1 is 3.6ltrs veg oil and other is 3.8 ltrs of used sunflower oil. I have also been trying to sorce a supply of used oil from some local businesses but they are all selling thier oil for betweet £5 and £6 for a 20 litre drum it is then exported.
Kind Regards to Both of you
Mark
-
Hi mark, no worries, just advance at your own pace, there is a lot to learn. It really short-cuts the learning curve if you visit someone local to you that has been making bio for a while.
-
Hi mark, saw your pm. Everything is 'above board' on here so I will reply on the main forum (there are several in infopop that poo poo the 2 stage no titration method which is why I kept quiet on there)
Here are a couple of links;
http://www.biopowered.co.uk/wiki/3/27_test
http://www.biopowered.co.uk/wiki/Two_stage_process_with_no_titration
Trouble with titrating is if you don't get it correct 1st time then you can end up with unconverted oil after conducting a 3/27 or 5/45 or 10/90 test (they are basically all the same test but as the 10/90 uses more sample it is the most accurate) in which case you have to use the result of the dropout test to calculate the chemicals for the next stage, so you may just as well use this result in the 1st place without titration. Once you have done a reaction you cannot re-titrate as the crude bio will be alkaline.
Just as a ps to this post, I used to do titrations for a living when I worked at ICI. I have never thought much of the waste oil titration for ffa's. The average colour of wvo doesn't help, making the mix with ipa quite murky. This coupled with a very wide endpoint, together with a fading endpoint makes these titrations more of an approximation than an accurate test. IMO.
Nearly forgot- on higher titrating oils the calculation of base + titration is not correct. After a titration of around 4 a more accurate calculation is base + titration x 1.2 The liberated water on higher titrating oils will increase the amount of chemicals required exponentially.
-
Hi All
Well I decided to go for it and make a 3.5 litre batch using some used vegi oil I have have for months. Here is my first attempt?
(https://www.photobox.co.uk/my/photo?album_id=5269922425&photo_id=500624436727)
-
Well done Mark, you have got good separation there.
-
Here's a test sample of unwashed Biodiesel using 50/50 soap test
-
A question Do I syphon the Biodiesel of the Glyserol and then wash or do I wash as is for the first wash?
-
Here's a test sample of unwashed Biodiesel using 50/50 soap test
Considering that is your crude bio then that isn't bad at all. You can't really do an accurate 50/50 until you have either de-methed by bubbling and settling or water washed.
Regard this 50/50 as your 1st water wash (on a small scale) try and separate the bio on the top and go again with the test. Repeat until the water layer is clear, the resultant bio would need drying to use it.
Do not try and wash the bio with the glycerol present, separate the bio first.
I don't think you have produced much soap with this small batch, otherwise your 50/50 would be total emulsion. Probably the reaction is slighty incomplete (producing less soap- this is where your 10/90 dropout tube is useful)
For a 1st go I think you have done really well.
-
Thank You Dave for the replies and encouragement.
Here is a 50/50 test after first wash.
-
That's good, see how much clearer the water layer is. Keep washing until it is totally clear. (it usually takes 4 to 5 washes) Don't worry that the bio layer is cloudy, it always is during and after water washing.
-
Hi All
I have just completed the 5th water wash now waiting for it to clear. I will then start reclaiming any biodiesel from the soap content.
So far the 3.5 Litre batch has produced about 2 litres of white soap can this be used for anything or is it just waste.
Kind Regards
Mark
-
Mark, add a small amount of acetic acid (vinegar) to the soap emulsion and mix it, if there is any bio tied up it will split into 2 layers with the bio at the top.
-
Thank You Dave for the tip with vinegar just managed to recover about 1 litre of biodiesel for washing. Does the white stuff have any use?
Kind Regards
Mark
-
The white stuff should be basically just soap and water.
-
Final wash completed.
Now for drying to remove water. I know some pf you prefer to bubble dry. But I do knot have a pump and air stone so any suggestions on how to dry please?
-
Warm to about 60degs and occasionally stir. Try it for a couple of hours. Using the 'clear and bright' test if indeed it is like that when cool then it is ok.
-
I seem to have reached the maximum number of pictures I can put up for this post. So before drying the oil was dull and cloudy after about 2 hours stirring every 10 minuets and allowing to cool it turned out clear and Bright. However on a 50/50 shake test using distilled water the water turned out slightly cloudy and the biodiesel was also dull and cloudy.
Have you heard of the 3/27 test, whereby using 27mils of Methanol you then dissolve 3mils biodiesel and the result should clear, it is ment to be a test for unreacted oil.
Regards
Mark
-
HI All
Here's an update the 50/50 shake test cleared after about 4 hours now crystal clear, I also carried out a 3/27 test after about 2 hours the test has I light yellowish tinge to it but no drop out.
Any advise please
Kind Regards
Mark
-
Hi Mark, I think thats 3x goods. One for the conversion (3/27) One for the 50/50 and one for the clear and bright bio.
The 3/27 conversion test is the same as the 10/90 (same proportions) but as the 10/90 uses more sample it is more accurate. I posted a link for the pictures of the 10/90 tube earlier in this thread.
Your 3/27 will have picked up some colour from the bio so that is normal.
-
Hi Mark, I've just seen your calculations on the 'American Channel'. there is something wrong with your working out (although I appreciate you have ended up with good biodiesel)
I don't really have time now to comment in full (going out) but you say your potassium is 99% pure. I think you will find it is 90% pure. When you add the titration amount it is per litre, not per the whole batch. Also when adjusting the amount of potassium for purity you should end up with a greater weight, not less.
Will reply later tonight, Cheers.
-
Hi Dave,
Thank You for pointing out my mistake on the other forum. I did check my calulations using the titration tool on here witch gave the same answer as my calculations 35grams of KOH, yes it is 98.99% pure I purchased it for another mod on my car witch works very well giving me fuel saving of around 20% around town and around 25% on a run. I hope we are not going to fall out over 0.01%.
Another 2 questions if I may
"how does one test for water content?"
"do I need to let a new batch stand or can it be used straight away?"
-
Hi Mark, I realise that analytical grade KOH can be more than 90% pure. It is just that for our use it is never used. The 90% works well enough (even though the missing 10% is water)
Just remember the titration amount of 2.1 is added as gms per litre, so in your case the actual amount was 7 + 2.1 x 3.5
ie 31.85gms
Your bio does not need to stand and can be used immediately.
Water is not easy to test for. The cheapest way is to build a manometer. Other methods , sandy brae and karl fisher are more accurate but very expensive.
https://www.youtube.com/watch?v=Gf-aoDHmKkc
-
Hi Dave
Thank You for the reply will make sure next I get cals right .
I see what you mean about the other web site.
Have you seen this and have any break throughs been made.
http://www.burnveg.com/forum/viewtopic.php?t=832
Kind Regards
Mark
-
Hi Mark,
julian (this forum) and myself have spent many a happy hour messing about with these sensors and we got nowhere, have a look here.
http://www.biopowered.co.uk/forum/index.php/topic,2494.0.html
Mark, after you mentioned your HHO unit in infopop it may be an idea to start a new thread on here, I'm sure quite a few would be interested.
-
Hi Dave
Thank You for the reply
After the responce I got from Tilly on Infopop I would need to give it some thought. I went to pick my wash and drying tank today needs a good clean and the outlet valve is blocked with mud. I will also have to check the heater and install an inlet port to circulate the biodiesel as well as a spray nozzle and plumbing.
I have not used my biodiesel yet due to my long run today so will put some in the tank tomorrow to see how my car runs on it around town. Not sure how a 2006 Citroen C5 1.6 HDI VTX+ fitted with the DV6 9HZ engine will take it. But It will be mixed with Diesel left in the tank from todays jurney.
Kind Regards
Mark
-
Hi Dave
Just been reading up on oil in water sensors and came across this I do not know if you have seen it?
http://www.iopscience.iop.org/article/10.1088/1742-6596/776/1/012118/pdf
Regards
Mark
-
Hi Mark, the link doesn't seem to work. >:(
-
Hi Dave Just Repair link
-
Highly interesting Mark, I wonder if Julian has seen this.
-
He has ... but unfortunately it's not dealing with measuring moisture content, it's monitoring level in a tank.
It's a similar theory to what we played with, but they are looking at way bigger changes in signal as the level travels up and down the sensor. Our sensor was fully immersed all the time and we were looking for minute changes in capacitance as the moisture content of the liquid changed.
-
Oh well, no worries.
-
Hi Dave
Thank you for the reply.
Can you tell me who is doing the "FOC water tests by Sandy brae or Karl Fischer for forum members." ?
Regards
Mark
-
It is my goodself, just let me know if you want to send a sample and I will pm you my details.
-
Hi Dave
Yes please what size sample do you need please?
Regards
Mark
-
A 100ml sample is fine. I have pm'd you my details.
-
Hi Dave
Just posted 100ml sample to you should arrive Monday or Tuesday.
Regards
Mark
-
Good, do you want me to post the results on this thread or pm them to you.
-
Hi Dave
Can you post them on the thread please. I have also just had a bit of luck on ebay just won an auction for 75 litres of methanol for £15.00 in Bexley about an hour away from me in the car.
Kind Regards
Mark
-
Here are your results Mark;
Appearance - clear and bright
Soap <10ppm
10/90 Warnqvist test 0.7mls dropout
Water 150ppm.
Comments - dropout test. The 10/90 test that most of us use is more accurate than the 3/27 as much more sample is used. When the tube was shaken the methanol phase was cloudy (that nearly always indicates an amount of unreacted oil)
The test can only be read when the methanol phase is clear.
Water test, although I repeated this I don't think from experience it is correct. It is possible that my Calcium Hydride is too old and not as reactive, sorry about that. I will order some more in the next few days.
-
Hi Dave
Thank You for running the tests for me.
Is this Biodiesel ok to use or do I need to process again?
Any comments from other members welcome.
Kind Regards
Mark
-
Generally the norm is to fully convert if using it in a modern common rail vehicle. If using in an older indirect injection the conversion isn't as critical.
I wouldn't hesitate to use it in either of my older vehicles.
Just on the subject of water, the spec is 500ppm. Most people don't water wash, so they assume there is no need to dry their bio. From many tests I have done this unwashed/undried bio is around 600ppm. My bio some 8 years ago was washed but not dried properly and was around 800ppm water. (I only realised this after getting my testing equipment)
Most samples I test are over the 500ppm limit ( hence my results on your sample being questionable)
To my knowledge no one has ever had any obvious problems using bio that is over spec on water. ( just to qualify this, biodiesel will hold dissolved water up to around 900/1000ppm depending on temperature. It is always this dissolved water we are referring to when talking about water tests, not free or suspended water)
-
Thank you for the reply Dave,
If other people did not water wash thier Biodiesel then how did they get the soap out, I water washed my test batch 7 times then dried in a 10 Litre pan over a low heat mixing about every 10 minuets I did this until I could not see any steam coming of the Biodiesel approx temp 55deg C and took about 50 minuets, So your water test could be right.
Any suggestions on completing the conversion process for the remaining 2.2 litres I have?
Mark
-
Hi Mark, there are various ways to dry wash, however it is best to start by getting rid of the methanol usually by bubbling with an aquarium bubbler for an extended period. The soaps and glycerine will then fall to the tank bottom and can be run off.
To reduce the soap further to below the spec of 66ppm one of the most common ways is to filter through hardwood shavings (oak is good)
You would have to re-process your remaining 2.2 litres to achieve full conversion, to make sure you convert it fully let's use a base of 8gms (I realise you have nearly 100% KOH so your base is actually 7.0)
0.7mls dropout = 7%, so 7% of 2.2 = 154mls of unconverted oil, so at 8gms/litre thats 1.23 gms KOH. Dissolve this in about 30 mls of methanol and re-process.
Remember you will have to go all through the wash/dry process again.
-
Thank You Dave
I will do that tomorrow.
Mark
-
Reprocessed the veg oil yesterday and has now been left for about 20 hours to stand, now showing a very small amount of Glyserol on the bottom. So will leave overnight again to see if the amount increases.
Mark
-
Hi All I have just purchased this Biodiesel Reactor of Ebay for £50.00 I could not build one for this.
-
Did you get everything in the picture? if so great deal, I can't see the pump, what pump has it got?
-
Well done Mark, great deal.
-
Hi All Thank You for the replies. Yes it is every thing in the picture but do not know what pump it has. Unfortunately I can not collect until Monday. So will let you know more once I have it.
Regards
Mark
-
Hi All
I have now finnished reprocessing my first batch water wash got abot 1.25 litres of soap again, Water washed until the wash water was crystal clear. Then dried over low heat to steam of water stirring every 10 minuets. Dave can I send another sample please for testing.
I am also about to start processing some Sunflower Oil I have dried and filtered this oil but have noticed that it is much thicker than the veg oil I have just completed. Do I need to make any adjustments for the thicker oil please?
Collecting Processor this Sunday so will update you on the pump type.
Kind Regards
Mark
-
Hi Mark, just send a sample when you wish. You shouldn't have to make any adjustments for the different viscosity of the oil. Just remember that the titration will be different so it will need a different amount of KOH. Better still, do a 2 stage process and use the result of the dropout after stage 1 to calculate your chemicals for stage 2.
-
Hi Dave
I have started processing next batch using 2 stage process. It is 3.6ltrs of sunflower oil split across 2 x 2ltr containers. I used the non-tritation calculator in the tools menu to work out the methoxide mix 300mls methanol and 8grams KOH for 1.6ltrs batch and 200mls methanol and 8grams KOH for 1.5ltr batch. These are at room temp, has been standing over night, I checked them this morning and I appear to have the Austrialian effect. Namely the Glyserol has risen to the top. Could this becaused by contaminated Methanol?
Kind Regards
Mark
-
I think I know what has happened here. Lets take the 1.6 litre batch, you have used about 19% methanol but only 5gms/litre of KOH (probably about half the amount you will need to fully convert bearing in mind your oil will have a titration, although unknown)
Because of this chemical imbalance the glycerol created will be so methanol rich it will not exceed the s/gravity of the bio/oil mixture, it therefore floats on top.
If I were you I would re-process using another 5gms of KOH in just enough methanol to dissolve it. Leave the glycerol in there and re mix.
You say the 2x batches were 1.5 and 1.6 litres but you used 3.6 litres of oil?
Cheers, Dave.
-
Hi Dave
Thank you for the reply. A typing error should be 3.1 litres total 1 batch 1.5ltrs 2nd batch 1.6ltrs will reprocess 1.6ltr batch with 30mltrs Methanol and 5grams KOH tomorrow.
Cheers Mark
-
Hi Dave
Yes that worked now have Glyserol at the bottom one for me to remember. Thank You
Cheers Mark