The Imsides method

[WesleyB Donating Member Find all posts View Profile Close WesleyB]

Re: Reduced oil temperature in reactor ?

Initially I put 13 grams calcium oxide + 11 grams 85% potassium hydroxide and 330 milliliters technical grade methanol into a 500 milliliter flask fitted for magnetic stirring. I made more methoxide solution than I would need. I stirred a bit from time to time to try to dissolve all the potassium hydroxide. Previously I tested new Mazola (name brand) corn oil for free fatty acids, I got 0.6 grams sodium hydroxide per litre to neutralize them. So I used magnesol XL to treat 700 milliliters of new corn oil thinking that might remove the free fatty acids (a small quantity). Eighteen hours (about) after I mixed the methoxide solution, I decanted off 100 milliliters of the upper clear liquid leaving the white solid in the mixing flask. I avoided putting the white solids into the vegetable oil. Mixing the 100 ml methoxide and 380 ml corn oil was done at room temperature of 22 degrees centigrade in a 1 litre glass storge bottle with a teflon cap. I shook it a few seconds , it separated that time. About one minute later I shook it a few seconds again, there was a noticeable color change and it did not separate quickly. Within about 15 minutes at room temperature a brownish glycerine layer was forming. The larger upper layer was transluscent. About 8 hours later I removed the glycerine layer in a separatory funnel ,then I washed (extracted) 5 times with distilled water. I got about 360 milliliters of wet biodiesel , added 40 grams anhydrous sodium sulfate (a drying agent). At 5PM the next day decanted off somewhat dried transluscent biodiesel. Added 25 grams magnesium silicate to remove more polar chemicals from the biodiesel with 60 degree centigrade heat on a hot plate with stirring. The biodiesel became transparent. Did a 10/90 Warnquest miscibility test there was no fall out. did a soap test but there seems to have been no soap in it at all, the biodiesel did not turn the bromophenol blue indicator blue for the test.

[smithy Senior Member Find all posts View Profile Close smithy]

Re: Reduced oil temperature in reactor ?

I did a test a while ago with magnesol + WVO

400mls of lightly used rapeseed oil that titrated at 1.0 with KOH. Added 3 teaspoons full of magnesol, heated to 50degs, stirred several times, left to cool and settle. Re-titrated with a result of 0.3

A residue layer appeared in the beaker not too dissimilar to glycerol.

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: Reduced oil temperature in reactor ?

Hi Wesley,
Thank you for the additional information.

You mixed 11g KOH into 330ml methanol and dried it with calcium oxide.
You did not titrate the new corn oil but you did mix magnasol in the new corn oil. Because you did not perform a before or after titration on the oil you have no idea what, if anything, the magnesol did.
My experience with titrating new veg oil is that it reaches titration end point with 1 or 2 drops of titrating fluid- virtually a 0 titration.
You then used 100ml of the dried methoxide to react 380ml of new Corn Oil..
Doing the calculations, that shows that your chemical usage was about 8.7g KOH per litre of veg oil and about 260ml methanol per litre of veg oil.

This is slightly more KOH than most people would use to perform a reaction on new Veg oil and substantially more methanol than most people would use to perform a reaction.
You performed the reaction at room temperature and eventually the biodiesel produced passed the warnqvest test.

Considering the quantity of KOH and Methanol used in the reaction, I would have been surprised if the biodiesel produced had not passes the Warnqvest test without drying the methoxide.
Did you have a specific reason for making this small batch of biodiesel?

[WesleyB Donating Member Find all posts View Profile Close WesleyB]

Re: Reduced oil temperature in reactor ?

I asked Dr Mark if his Imisides Method (using cement) passed the 10/90 Warnquest miscibility test. I got no answer, so I tested some cold method biodiesel I made using calcium oxide. I could not find that lab note book. It may have walked off or something. Loosing a lab notebook is a problem since I usually can't rely on my memory from September of 2017. So I did it again with writing down what I did in another lab notebook. Generally in synthetic fuel production it's important to use less energy to make it than is harvested from it when it burns. So developing a practical, working room temperature synthesis pursues a goal of making energy inexpensive synthetic fuel (biodiesel). That's part of why I did it. Dr Mark didn't answer the question, so I did. My take on this Imisides Method does pass the Warnquest miscibility test and has little soap in it. I couldn't detect any soap using the Bromophenol Blue pH indicator test.

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: Reduced oil temperature in reactor ?

Hi Wesley,

So developing a practical, working room temperature synthesis pursues a goal of making energy inexpensive synthetic fuel (biodiesel)

This is the part I do not understand.
It has been repeatedly shown to you that you can make biodiesel at room temperature using the standard method. No CaO or any other methoxide drying procedure is required. People have been doing it for years!!
For some reason both you and Mark continually ignore this fact and tell everyone you are on this noble quest in search of a magical procedure that allows you to make biodiesel at room temperature.
The procedure already exists! It has existed for years!!!
Just use your normal method of making biodiesel and do not heat the oil. As long as the oil remains liquid you can mke biodiesel that passes the Warnqvest test.

That's part of why I did it. Dr Mark didn't answer the question, so I did. My take on this Imisides Method does pass the Warnquest miscibility test and has little soap in it. I couldn't detect any soap using the Bromophenol Blue pH indicator test.

You did not use the Imisides method. You did not even come close. Go read it again.
1. The instructions for the imisides method say to dry the methoxide with cement powder. You used CaO to dry the methoxide. Cement powder and CaO are not the same thing.
2. The instructions say to use use 15g KOH per litre of Veg Oil. You used 8.7g KOH per litre of Veg Oil
3. Mark has just increased the methanol from 15% to 20%. You used 26%
4. There is no mention of the magnesol treatment of the Veg oil that you used.
About the only similarity between the imisides method and what you did was to not heat the veg oil, everything else was different.

And at the end of the day, because you were reacting new Veg oil with such a large excess of chemicals, all you needed to do was mix the Methoxide with the room temperature Veg Oil and you would have easily passed the Warnqvest test, No methoxide drying required.

[WesleyB Donating Member Find all posts View Profile Close WesleyB]

Re: Reduced oil temperature in reactor ?

Well Tilly you're right. I reacted 380 milliliters Mazola new corn oil , titration number 0.13 with 100 milliliters methanol with 3.4 grams 85% potassium hydroxide dissolved in it, at a room temperature of twenty five degrees celcius, with stirrirng over a period of 8 hours to get a glycerine layer. Removed the glycerine layer. 8 hours later washed 5 times with distilled water. Dried the biodiesel over night with 30 grams anhydrous sodium sulfate. Removed the sodium sulfate drying agent. Heated to 60 degrees Centigrade then added 16 grams magnesium silicate with stirring, left to settle over night. Decanted the purified biodiesel off the magnesium silicate and did a Warnquest 10/90 test, there was no fallout. So, biodiesel transesterification reaction can be done without heating using the regular method.

[Dr Mark Senior Member Find all posts View Profile Close Dr Mark]

Re: Reduced oil temperature in reactor ?

Done some quantitative measurements on this:

The vol% of my MeOH is about 17%. (20/120). After conversion, this equates to about 22% (v/v) glycerol. I never did any quantitative measurements with the previous ratios, but I'm pretty sure that this is a higher ratio, which is what I'd expect

Hi Guys
I've made a mod to this method after some quantitative measurements. I've decided tu increase the methoxide ratio from 100:15 to 100:20. This accounts for the amount of MeOH that is consumed by the drying process - something I'd never measured before. In fact the leftover meOH was probably below the stoichiometric amount. With the old ratio of 100:15 it's likely that I wasn't getting complete conversion and there was probably a significant amount of unreacted WVO in there.

With the new quantities I'm getting more glycerol, and it's taking longer to remove the MeOH, so I'm sure it's now fully converted.

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: Reduced oil temperature in reactor ?

Hi Mark,

I've decided tu increase the methoxide ratio from 100:15 to 100:20. This accounts for the amount of MeOH that is consumed by the drying process ...The vol% of my MeOH is about 17%. (20/120)

Wow, so your procedure of mixing cement with the methoxide is removing 30ml methanol from the reaction for every 200ml of methanol you use. That is 15% of your methanol going down the drain! What an expensive waste.

After conversion, this equates to about 22% (v/v) glycerol. I never did any quantitative measurements with the previous ratios, but I'm pretty sure that this is a higher ratio, which is what I'd expect

Yes, it was obvious that you had never performed any quantitative measurements on your procedure. Otherwise you would have realized years ago that the original procedure you posted would not produce very high conversion biodiesel.
Of course measuring the amount of by-produce/ glycerol is not a meaningful indicator of the quality of the biodiesel produced. There are many variables that will affect the amount of by-product produced.
Your increasing the amount of methanol used in the reaction will result in an increase in the quantity of the by-product layer for the simple reason there will be more methanol in the byproduct layer.

If you require any further help please let me know

[Dr Mark Senior Member Find all posts View Profile Close Dr Mark]

Re: Reduced oil temperature in reactor ?

One more thing that I've noticed - with the previous ratio of 100:15 for the MeO I was getting a bit of a smoky exhaust when the engine was idling when cold (with my Merc). With the new ratio of 100:20 it has now disappeared. This confirms my belief that with the the 100:15 ratio there was still a significant amount of unconverted triglyceride left over.