It is clay.
Ive been looking everywhere and i cant seem to find an answer to how im suppose to wash distillate in water.
I dont want to be spoon fed, i have my own spoon, i just dont know where the bowl is…
1 Like
Just stir it up gently between 70-90°C, with the distilate+clay on top.
The clay should progressively sink in the water layer.
1 Like
Is this what you are referring to?
The water wont contaminate the distillate? This is when a seperatory funnel is utilized?
That can work. Our old trick was just a stainless steel scrubbie from the grocery store
2 Likes
You’re going to have a hard time using a separator funnel at such temperature, unless you first mix your distillate in a non polar solvent such as heptane or so to perform the same at room temp… then you will have to remove the heptane.
If you proceed as I said, using a reactor which you can heat, and drain from bottom, you could just let it cool down until the distillate harden, and rapidly drain the water from below. Then heat up again and dry the distillate with some molecular sieve.
1 Like
Okay, thank you i really appreciate the clarification!
When distillate and water are mixed in that manner, the distillate settles on top, allowing the clay to fall to the water below?
Are you referring to a piece of equipment like this?
https://www.amazon.com/dp/B07F6SGK79/ref=cm_sw_r_cp_api_i_Yv1.EbYR3SPY1
Thank you for demistifying this for me.
It’s not much harder to use a seperatory funnel. Keep in mind you should be doing multiple washes. So even if you use a reactor with a drain you will have to refill it for each wash.
Also, please do not skip vacuum filtering your product to remove solids first.
It sounds to me like you could use a more thorough SOP
1 Like
You are already playing arround with a distillator and hot liquids. Just try mixing hot distilate with hot water and see how it behaves. Pretty sure you will figure out a convenient method quickly!
That reactor here looks convenient. You need something jacketed that you can easily stir and drain.
1 Like
Thank you
Easiest way I’ve found to remedy this is to pack your columns when distilling and don’t let the mantle temp get too hot. I agree with what BreakingDabs has suggested with the steel wool at the store. Lightly pack it and it will help prevent a lot of particles from climbing up your fractionating column. It probably already has indentations in it to help prevent some of it but packing it yourself further prevents it. The steel wool has worked well for me.
1 Like
At that size that reactor is overkill. Magnetic stirring shouldn’t be an issue in a 1 liter flask as long as you’re refluxing in solvent. You’ll need to add solvent later for water washes anyways, and you’ll get better yields with your clay reflux in a solvent. A seperatory funnel is going to run you less than $100.
I would have to then use a rotovap to get rid of the solvent, then redistill correct?
So i can put this in a funnel, and run my distillate through this to remove all water after water washes? This is absolutely fascinating.
Use this only once water is present as traces in your distillate, at the very end.
This will dry it out. I would not use it in a sieve (too coarse). I would rather throw a bunch in disty (mind rinsing them from their powder first), and keep it 60°C for a while, with occasional stirring. Then I would remove them with a strainer or a coarse sieve.
Thank you.
1 Like
Use zeolite to dry out extracts while they’re in solution. This dries out the solvent and the solute. From there you evaporate your solvent to yield a dry extract.
@awkwardballer I sent you a dm, I can walk you through all this
4 Likes