Help! Following Noman: fibers into the lye or not?

[alexcycling]

After searching, I concluded discussing extraction is legit here. If not, please inform me.

I follow noman's tek (and yes I have some experience with chemistry and know how to handle NaOH and acids etc.).

I need to start from chunked stuff, and 'treated' it with a high-speed mixer which resulted in powder and fibers. I tried to run the fibers through a decent coffee grinder, but it gets stuck (as I expected), so I'm left with powder/fiber mix.

The text (addendum 1) also comments on the pre-powdered stuff: it has at least a part of the fibers also powdered, which leads to a sludge which won't release the naphta. From this I conclude we should probably not have the fibers in the solution? But I guess that keeping the fibers there might extract extra good (or bad?) stuff. And: separation of the powder from the fiber is impossible; so getting rid of the fibers in dry state would mean to also remove lots of powder.

So the question is how to proceed?
Having fibrous stuff in the solution makes it hard to separate the phases later on using a separation funnel. Getting rid of it from the lye phase before adding naphta is nasty (e.g. filtrating the alkaline stuff adds extra complexity / dangers).

So would one leave it all in and go for an Erlenmeyer flask / pipette approach?

Another question is:
I'm thinking about using some water in the mixer, as this might help braking down even further. Then decanting everything into the actual mixing jar and carfully adding NaOH.

Any thoughts?

 

[reverse cosmosis]

Some tips based on experience.

Leave the fibers in but use a Mason jar, not an erlhenmeyer. The shape of the erlhenmeyer seems to contribute towards emulsification issues.

If your solution emulsifies heat it to roughly 40C (or equivalent in freedom units) and periodically rap on the glass with your knuckles.

It's worth marking your levels before and after adding NPS so you know how much you've got back from solution. 90% return is fine.

If all else fails walk away, smoke a doobie and forget about it for an hour. By the time you come back 95%+ of your NPS will have been released from the emulsion.

If your solution is really sludgy try adding more water while maintaining a pH of 13+.

Sometimes adding more NaOH or NaCl can help release an emulsion too but it's usually not necessary as long as your original solution was watery enough and pH13+

 

[reverse cosmosis]

Another tip if you're having trouble breaking down your source material fine enough is freeze the material before you blend it to make it more brittle.

Then after blending add it to a slightly acidic water solution and freeze/thaw cycle it a few times.

Nomans tek is simple but it's pretty old now and leaves out a lot of the knowledge gained since then. Cyb's hybrid ATB or Max Ion teks describe these processes in detail and ime give more reliable results.

 

[alexcycling]

OK, thanks for the hints.

 

[alexcycling]

I now added the water to the dry stuff in the blender and let it run for a while, gets things much smaller.
The smoothie is now freezing.

There is also vovin's tek adding an extra washing the naphta with sodium carbonate water. This sound sensible to me, as it gets rid of NaOH which might have made it into the NPS (nonpolar solvent).
Any experience with adding this step to Max Ion?

And my version of Max Ion states to heat to low heat, the glas vessel should be able to be handled without burning). So this is ~45°?

 

[reverse cosmosis]

I had one dirty looking batch of NPS I did a sodium carbonate wash on but generally I just let it settle and it seems clean enough to siphon off the top with a pipette. Never hurts to clean up though.

As I'm sure you already know the wash is done after pulling and before freezing. Its a lot simpler to separate as it doesn't form an emulsion too.

 

[alexcycling]

I had one dirty looking batch of NPS I did a sodium carbonate wash on but generally I just let it settle and it seems clean enough to siphon off the top with a pipette. Never hurts to clean up though.

As I'm sure you already know the wash is done after pulling and before freezing. Its a lot simpler to separate as it doesn't form an emulsion too.

Yes, I have seen and also thought its quite simple and could be worth it.