LLE question? Heptane/methanol/water

[tweedledew]

Shoot, I was reading his old Tek. His newer one seems way easier.

[ToOmUcH]

Hey you ever considered carbon scrub after decarb to lose less d8? If short path is your end goal

[Roguelab]

Wich one ?

[ToOmUcH]

@Kingofthekush420

Dissolve 8:1 I’m methanol, carbon scrub, degum, and clay scrub, winterize, then I do the heptane washes till the heptane comes out clear. Roto vap the heptane and 2 passes you’re done

this one

[Kingofthekush420]

@ToOmUcH

Hey you ever considered carbon scrub after decarb to lose less d8? If short path is your end goal

If spd is your main goal then yes decarb before carbon scrubbing

[tweedledew]

Ok…
New plan…

As per this:

LLE second test

I wonder if one could extract the terpenes out of that aqueous solution without destroying/degrading the terpenes?

I will take my winterized methanol solution (6L) holding (approx 1000g of oleo)

Put it into a 30L separatory funnel

Add 2000ml heptane & stir

Slowly add in water until layers start forming, dumping off the lower water+meth layers

Allow it to run clear.

Does this sound better?

I’ll probably take the methanol+water layer and run a pentane wash if it’s got any nice terps in there.

[munkdooligan]

@tweedledew how has this been working out for you?

We are getting our chromatography setup this week and we’ll have some fractions with methanol and water. I think doing an LLE like you are doing might be a better way of recovering the cannabinoids rather than straight evap.

[tweedledew]

I’ve been doing lots of LLE just to play around.

The pH degummimg technique is useful for warm extracted or hydrocarbon crude.

Doing salt water washes is good for removing some of the reds in an ethanol crude.

LLE is certainly useful on the whole though

[Rowan]

would this alkane pulls post methanol winterization work with pentane? its all I have on hand rn also this is on hemp crude

[BrotanicalMatt]

Why do you carbon scrub first? Dont the other pigments compete for space on the active sites?

[NoHeatNoVacuum]

I’m gonna go slightly out on a limb and say yes, with some possible slight parameter changes from slight differences in properties. So I imagine you are more interested in CBD since it’s coming from hemp?

[Rowan]

goal is a nice rtg crude oil

[Kingofthekush420]

@BrotanicalMatt

Why do you carbon scrub first? Dont the other pigments compete for space on the active sites?

When I’m doing liquid liquid its for pigment removal. Carbon is just an extra step to help remove more color than liquid liquid alone.

[BrotanicalMatt]

Yes but what i’m asking is your carbon scrub your first proportional step? then clay etc.

If it is your first step - what is your reasoning behind that?

[Kingofthekush420]

@BrotanicalMatt

Yes but what i’m asking is your carbon scrub your first proportional step? then clay etc.

If it is your first step - what is your reasoning behind that?

Efficiency, I’m not going to winterize or do first pass then have to refilter.

[Rowan]

I’ve been doing clay and AC at the same time, the follow with DGC and water wash- then dissolve 2:1 pentane/oleo and water wash as per the CC SOP

I’m thinking to just get rid of the water wash step, instead dissolve the hot scrubbed and degummed oleo in methanol, winterize, then pull with pentane. sound good?

[BrotanicalMatt]

Have you done a freundlich isotherm to calculate the efficiencies/equilibriums of the solutes absorbed by absorbant? My humble opinion with our refineries is more or less is the proportional steps taken and the efficiency that compounds with each step. Saves a-lot of money and time - economies of scale.

In short…even tho you are trying to removing any impurity - pigments, etc - they each have a chemical benefit or baggage involved at certain steps in the process.

[BrotanicalMatt]

I think both ways are pretty good - if you want i can look in depth on the one you are thinking about. I personally like water. There is alot you can do with it. Cheap and easy.

[Kingofthekush420]

@BrotanicalMatt

Have you done a freundlich isotherm to calculate the efficiencies/equilibriums of the solutes absorbed by absorbant? My humble opinion with our refineries is more or less is the proportional steps taken and the efficiency that compounds with each step. Saves a-lot of money and time - economies of scale.

In short…even tho you are trying to removing any impurity - pigments, etc - they each have a chemical benefit or baggage involved at certain steps in the process.

Tbh I’m not exactly sure what you’re trying to say or what your point is.

I’ve done side by side comparisons on the same material and the scrubbed material is always light because of less bandwidth.

I can take warm extracted alcohol crude and make it just about water clear with this SOP ( I developed the one I posted above ) several ppl here have used this to fix messed up colored distillate without Clay’s in the flask or chromatography.

It works, it might not be “optimal” but for efficiency it is, and someone who wants “optimal” isnt going extract with warm alcohol for extraction. I only use this on warm extracted alcohol crude.

[BrotanicalMatt]

If you carbon scrub first you are removing tocopherols. They stablize oil at least in “harsher” environments. You are also discounting the phospholipids that compete for space with the chloroplast on binding sites. Thus when you have reactors that need one ton of absorbants it is in your best interest to be efficient. All my question was is what is the reasoning behind it AC first.

But what do i know! my 2 cent.