Ethanol Heptane Seperation

Mol sieves are not an option for recovery and volume of molsieves is gona be $$$$
In solvent loss

I tought of an Cartrige like i mentioned above.
https://www.m-chemical.co.jp/en/products/departments/mcc/ifm/product/1201039_9112.html
==> Only ethanol goes trough that membrane

44.4 % ethanol needs 55.5% heptane to form the azeotrope
So everything beyond 55.5 % is left of heptane in the flask
Say 1 liter of oil is 0.3% thc in 10 liter of etho adding 25 liters of heptane will give 24 liter azeotrope etho/heptane
And 11 heptane and 1 liter oil in solution example

Extract in heptane or etho/heptane straight ???:thinking:

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Membranes are an answer but a certain volume is nesesary to make the unit work and they are $$$$

My planed Unit are 80L Centrifugal Extractor and a 120L double walled tank for cooling. (I run a few baches with the same ethanol. My raw material hasnt that much CBD) With cooled ethanol my first tests had about 62% CBD.
This will be winterised and filtered.
Now i have a 100L distillery which can handle vacuum. Now i could drive this thing 3 times or i do it with mole sieve membrane. 100L should be enough for membranes.
Much less energy and time would be needed.
But in the end i have to seperate Ethanol Heptane anyways, except I extract with ethanol heptane mixture.
Ethanol Heptane mixture would be nice. It lowers the total amount of heptane. But the heptane dissolves the waxes and winterisation isnt possible !? I am right ?

You winterize treu a membrane

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Yes with celite 545. Is it still possible with cooled ethanol/heptane ? I don´t know exactly but i think i saw a post where it is said that the fats wont get cought when dissolved in heptane?

Search bar. Reverse osmosis

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I used heptane just fine in louching. It doesn’t like water, and when you add water to the alcohol you’re gonna get separation just fine. The ethanol loves water much more than it loves heptane.

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This is awesome.
Which pore size do you use that only and all cannabinoids pass trough?

Search bar. Reverse osmosis.

Or else DM and pay the man already if you want to be spoon fed.

Cannabinoids are big 314 dalton so use a smaller size to let it all go treu and keep the noids

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So when the Ethanol azetrope is saturated (maybe a bit more water), the cannabinoids fall out. Now i will put so much heptane into the water/ethanol that the crude THC content will be under 0.3% (if only heptane left)
Is the order important (for example: heptane first and then water) or is the ethanol water azetrope so much stronger that ethanol “goes” to the water an leaves the heptane.

Please forgive me if a chemist has an attack now.
I should get myself i chemist to help me out ^^

==>Most of the serpation can be done by an separating funnel??

Relax he s family now :wink:
@Weederlich. @MagisterChemist @Kingofthekush420

Ok so @Weederlich has an isseu that the law states at no time there should be 0.3% of thc present and has high hopes for the thc remediation tech of partial decarboxilation and molsieves
@Termite disclosed a bit
Got me thinking

A extract in heptane
B winterize in heptane by RO
C recover heptane treu RO till 0.3% thc mark
D partially decarboxilate while in solution of heptane under pressure
( prv installed)
E run over sieves till saturation of 0.3% then swap sieves
F recover all solvent
G distill as usual

Don t think it makes sense to USA extractors but in Europe it might
But other than that let’s yust stir the pot and contemplate on can it be done
Thx

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THANK YOU !!!
RO Membrane was the piece of the puzzle i was searching for !!!
That was the way i tought of (from D to G)
If I could i would give 100 likes!
I will experiment in that direction. For the next 2 days i will learn everyhing about RO.

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@tweedledew has it

If you do the process correctly you’d not really have to distill anything other than you ethanol/water mix which might have trace heptane in it. So the azeotrope is not really a factor. As Rowan said, the system is simpler with MeOH but I understand the reservations with using it.

Basically, just dump your EtOH micelle stream (reduced in volume will make your life easier) into a sep funnel/reactor, then add you virgin Heptane, then add water and agitate until you’ve diluted the EtOH down to 5-15% (someone who uses EtOH for this should chime in as far as optimal filition, I use MeOH). Then pour off your aqueous layer to be reproofed and collect your Heptane.

When you go to reproof the EtOH/water/heptane, you’ll only have a small amount of heptane in the material, which if you distill off first as the ternary azeotrope, you can just keep adding to your system each batch. This volume is “held up” but as like long as you hang on to it, is the only “waste” solvent.

You can also wash your azeotrope with more water to wash the EtOH out of the heptane and then dry the heptane. If you care to save that little bit. You technically don’t lose the EtOH but the biggest issue with this approach is how much alcohol you need to redistill from low proof.

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Hi there,

i haven`t read the threads above, but in our company if we have a azeotropic Mixture we normally change the pressure within the distillation column. We usually had about 2 bar in our bubble tray column.
Or you could also try to freeze one the solvent with the higher freezing point.
Ethanol -114°C
Heptane - 90.55°C
Should work with the difference.

I hope this helps.

The link below is in German.

(stgr + F—>HEPTAN ETHANOL about page 55) you`ll find some states about different mixtures of heptane and ethanol.

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