Is anyone else getting really tired of all the pedantic bullsh*t, ego posturing and petty squabbling and that has infected this corner of the forum lately? I'd like to ask people to get back to the good willed, generous natured sharing, and supportive critic that used to make this section of the forum a pleasure to be a part of and read.
Womble and Imake.
You have a private message.
Don't feed the troll put him on your ignore list and problem solved!
" 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.
imakebiodiesel; The biodiesel I made from beef fat was yellow and cloudy, for about 24 hours, after removing the glycerine layer, at 20 degrees centigrade.
After about 24 hours some liquid precipitated in the storage bottle (more glycerine + soap?), and the upper layer biodiesel became transparent.
I decanted off the clear yellow transparent biodiesel , leaving behind the lower liquid layer.
I put the biodiesel into a vacuum still, still pot. Distilled of methanol. I'm not sure how much methanol I was able to distill off as my condenser water was not iced. I probably pulled a bit of the methanol through and out of the diaphram vacuum pump.
I only got about 40 millilitres of distillate (probably methanol).
The still bottom became hazy/ cloudy, where it was transparent before demething.
While the still bottom was still warm, about 63-70 degrees centigrade, I added 20 grams magnesium silicate with magnetic stirring at 63-70 degrees centigrade, for about 45 minutes.
Turned off the magnetic stirring hot plate, and let most of the powder magnesium silicate settle out of the demethed biodiesel.
Decanted off about 700-800 millilitres of cloudy biodiesel into a 1 litre clear glass storage bottle with a teflon lined cap.
I am now waiting for what ever is making the biodiesel cloudy to settle out, at around/about 20 degrees centigrade.
I didn't water wash it. I didn't want to possibly loose part of my product to hot distilled water.
I'm dry washing it. How do you measure cloud & gel point accurately?
Wesley, the layer that formed after you removed the glycerol is most likely HMPEs with perhaps soaps as well, if it had been glycerol the colour would have been very recognizable. Hmpes will normally be cream to light brown colour.
If you put HMPEs into a glass beaker and warm them they will turn golden and clear.
Normally I test for cloud and gel point in the fridge and freezer. I fill a clear glass bottle with biodiesel and I tape a k type temp probe to the side of the bottle and then tape a thick patch of insulation material over the probe. I put it in the fridge and watch the temp fall. Every 2 degrees I take the bottle out , wipe it clear of condensation and look for clouding. If its still clear I shake the bottle and put it back in.
This method is not going to work for tallow biodiesel so here is my idea. Get a box about the size of a shoe box and line it with several layers of newspaper for insulation. Instal a light bulb as a heater and put the glass bottle in with the temp probe. Put a sheet of glass on top as a lid.
Use the lightbulb to heat the bio to say 50°C and then allow it to cool slowly. Observe the newsprint thought the bottle of bio and when it becomes difficult to read you have reached the cloud point. When it begins to thicken you have reached the gel point.
Incidentally the CFPP ( cold filter plugging point) is usually half way between the cloud point and the gelpoint.
Thank you for your replies to my PM, Ill study them today.
Tallowman, thanks for the sample of your tallow. Its certainly very white and clean. Ill have a go at processing at the weekend.
The joint between the polypropylene cap and the brass nut feels strong but what I find happens is the liquid, especially oil, will creep between the surfaces and eventually the joint will part. Still its fine for a short term connection but I wouldnt subject it to too much pressure.
By the way thanks for the tip about the € sign.
Ronny; I added magnesium silicate to dry wash my 700-800 milliliters of biodiesel made from beef tallow.
I read that Magnesol claimed it could dry wash biodiesel well. I think Magnesol was made of magnesium silicate.
I'm trying not to add water to my biodiesel when I purify it. I figure if I don't put water into the biodiesel, it avoids complications and expense in perfectly drying it.
I think magnesium silicate absorbs soap from the biodiesel. Then the powder magnesium silicate is removed. In this way adding water to my biodiesel might be avoided.
I recogise I might be wrong. I haven't done much quality control testing.
Magnesium silicate (Magnesol) has been used to dry wash and remove water from bodiesel, it's a white talc like powder.
I was given some a few years back by a visiting English man who funny enough originally bought it from a northern ireland company called minstrel chemicals.
I was worried about the fine talc like powder getting past the filters and causing wear to the engine but this was just my personal view.
The guy who gave me it had used it for years without problems.
Thanks IMB and Ronny for the feed-back
I have made a new 1 litre processor from a stainless steel dish.
12 inches = 1 foot = 305 mil
Depth = 150 mil
Length = 260 mil
Width = 145 mil
Cover = 295 mil x 145 mil
It is rectangular in shape and filled to maximum is almost 4 litre.
It is ideal for 2 to 2.5 litre batches.
So with my angle grinder I cut a concrete lintle to fill up 50% of the dish so I would have a greater volume to paddle mix; my 1 litre batch ;if I did;nt it would be too shallow.
The stainless steel cover is off another dish and is 35 mil longer than I need; but all the extra space allowed me to bolt a threaded bar onto it which holds my Methoxide bottle.
I can now administer the Methoxide in drip fashion without being present.
Onto the same cover I have bolted a small block of iron (on the inside) so I can allow the spear of my probe thermometer to remain firmly in place throughout the mixing process.
My hot-plate is taking a while to get used to ; I have been using water to experiment with;
first I heat it quickly on the gas flame to 60'C then (on the hot-plate) I try to keep it from going over 64'C .
at the moment it is staying between 62'C and 63'C for the past 5 hours so I am happy I have mastered it.
I will be using it in the next few days and will let you know the result
Sounds good Tallowman, good luck with it. |If I get a few hours this week I might process your tallow sample and do a few tests to the biodiesel.
Especially when heating potentially flammable materials I use a "sparkless hotplate". That is normal chemistry equipment.
I titrated the beef tallow in a 50 millilitre beaker. 1 millilitre tallow + 10 millilitres 91% isopropyl alcohol + phenolthalein pH indicator solution + enough 0.05 Normal aqueous sodium hydroxide solution. At room temperature, the tallow became a solid in the test liquid, So using a cigarette lighter I heated the test mixture up enough to melt the beef tallow, in order to get a NaOH titration number. The tallow needs to be a liquid during titration for free fatty acid content.
I have today received in the post a tank belt heater from China; which IMB brought my attention to 21 days ago; it seems to be of high quality.
If anyone is interested in an item of some sort on the Web ( ie. belt heaters; biodiesel Processor; water heater thermometers ; etc ; ) type it up and then go to the top left side of your screen and press the "Image" button and it will reveal hundreds of them with information on how to obtain them.
I am content to remain with my 1 litre processor until I can pass the 30/270 test at 20'C
Then I intend to use a stainless steel saw-steriliser as a 3 gallon processor.
I intend to mix using a circulation pump with an Eductor.
I will take Rickdatech advice and insulate; insulate; insulate .
Then when I have a complete master of the skill of washing/drying and have quality usuable fuel I will return to using my 120 litre cone shaped processor.
I think your approach is a sensible one. You learn a lot when doing small batches and at that scale mistakes dont turn into disasters. Some one very generously gave me a combined hotplate and magnetic mixer recently. I have ordered a 2 litre glass beaker and a set of magnetic stirrer bars to go with it. These should arrive this week and I intend to do a series of small tallow batches with this new gear.
The methyl biodiesel that I made from beef tallow does not perfectly pass the 3/27 test. So, possibly when rendering the beef fat, I might not have boiled enough water out of the hot grease. I've described above in this thread my proceedure. In the past week of the biodiesel settling, a transluscent 1-2 centimeters of a white material has settled out in the 1 litre clear glass storage bottle, with a teflon lined cap. The upper part of the biodiesel is now transparent bright yellow at about 20 degrees centigrade. This methyl biodiesel from rendered beef tallow is almost the same colour as biodiesel made from new corn oil.
My combination hot plate and magnetic mixer is a very useful tool, my thanks to Tony who gave it to me,
I put a litre of tallowmans tallow into a beaker and heated it to 60°C. the titration was 3ml KOH so I added 200ml of methanol and 11gms of KOH and mixed for 1 hr. I then let it settle for 1hr and carefully poured off the biodiesel. The bio was a pale gold and the glycerol was a mid brown.
I returned the bio to the hotplate and heated it to 105°C with the lid off and the mixer going vigorously for 1 hr. This would have demethed, and hopefully dewatered the bio. I realize that it may have caused a little oxidation but Im not concerned with that in this sample.
I divided the bio into 3 [portions , The first (left in the picture) has nothing added. The one in the centre of the picture has 50% diesel added and the one on the right has 20% petrol. The temperature at the time of this picture is 10°C.
The 50/50 diesel sample has resisted forming HMPEs very sucessfully. Its less than the picture suggests, these are wine bottles and there is a raised glass dimple in the base of the bottle. I would estimate that there is only 10% HMPEs.This message has been edited. Last edited by: imakebiodiesel,
To take the experiments a bit further I will settle these samples for a week to let all hmpes and soaps settle out and then I will test for conversion, water content and soap content. Once I have these tests done I should be able to propose a method of doing a 100 litre batch in a conventional biodiesel processor with very little additional equipment.
In the meantime I want to repeat the process with NaOH. I dont know if it is true but some sources claim that NaOH is better for tallow, we shall see.
To keep these tests consistent I want to use the same tallow if possible. Tallow man, would it be possible to send me another litre of your tallow? I would be happy to pay the postage costs.
Ive posted another picture of my 50/50 sample. The temperature in my store room is still 10°C and the other two samples have remained unchanged. The 50/50 sample has cleared considerably and the hmpes have settled lower in the jar.
The total depth of liquid in the bottle is 17cm which means that the total depth of biodiesel is 8.5 cm. The depth of the hmpes is 2 cm but as you can see from the empty bottle on the left about half of that volume is the glass dimple. So I estimate that the hmpes account for 12-15 % of the total volume of the biodiesel.
In the other sample the hmpes account for over 90% of the total volume.This message has been edited. Last edited by: imakebiodiesel,
I've got an old organic chemistry book that gives a list of the percentages of free fatty acids in beef tallow. There is 0.4-1% eicosanoic acid, a 20 carbon chain. When converted to the methyl ester it has a melting point of 45-48 degrees centigrade. Next is a saturated carbon chain with 18 carbons, that when converted to the methyl ester has a melting point of 31-35 degrees centigrade (stearic acid), methyl stearate, stearic acid methyl ester. I expect these are the high melting point esters (HMPEs) in the biodiesel derived from beef tallow. If you heat your biodiesel to 105 degrees centigrade while bubbling air through it from an aquarium air pump you might demeth better and dewater better to get a purer product. With a magnetic stirring hot plate you can heat a test batch up to maybe 170 degrees centigrade if you need to.
Wesley, my demething/dewatering method was rudimentary but quite effective. I tested some of the 50/50 batch with my carbide manometer and got a result of 170ppm which is acceptable for diesel fuel. Of course that doesnt tell me how much water was in the biodiesel because dont know how dry the diesel was. I cant test the other samples because they are solid at todays temperatures 15°C, I can turn the bottles upside down and nothing comes out.
In a larger scale processor I will be able to use my turbo dryer which bubbles predried air through the warm biodiesel and a fan that clears the headspace. This will dry any fuel down to the 100 ppm region.
I understand that the longer the carbon chain of the lipid and the methyl ester ,the higher the melting point and that the three samples contain the same mix of esters, excluding the diesel and petrol. However the pictures show clearly that far smaller proportion of these esters have crystallized in the 50/50 sample. My guess is that the winterizing agents added to the diesel at the refinery have suppressed crystal formation in the 50/50 sample. It would be interesting to find out what additives the oil companies use to winterize their diesel.
I warmed a small amount of the tallow biodiesel and performed the 30/270 conversion test today. The result was 98% conversion which I am quite happy with considering it was only single stage processing. I wont test for soaps yet as I think it will take at least a week to settle out the soaps.
I feel ready to suggest a procedure for a full sized batch for tallowman or any anyone else who is going down this route. This procedure is based on my own IMB150 processor and may need to be adjusted to suit other processors.
100 litres of warm liquid tallow is pumped from the boiler into the processor and heated to 64°C.
The tallow is titrated using warm tumeric/isopropyl.
The methoxide is mixed accordingly.
2 stage processing is carried out in the normal way.
Glycerol from the 2nd stage is allowed to settle for 2 hours and then removed.
The biodiesel is reheated to 64° and dried using the turbo dryer for 6 hours.
The biodiesel is transferred to the cold filter tank and mixed with an equal amount of petro diesel.
The mixture settles for one week.
Crystallized hmpes are drained off through the 2" valve and transferred to a heated storage tank and used as home heating oil. These hmpes will be contaminated with soap but that will make little difference to a burner.
Clear liquid biodiesel can then be drained through the 3/4" standpipe, filtered and used as motor fuel.
Here is a diagram of a cold filtering tank.
Tallowman if you would be interested in a trip down to Lismore you could bring 100 litres of your tallow and we could do a batch in this way. I can easily make up a cold filtering tank. I think this way you would see what you need to do to your own processor to get it working.
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