Hexane Honey Oil extraction and alchemy

DankTankUSA · May 27, 2012

G.O. Joe said:
I haven't seen anything, including their website, that says that their patent, or CO2 extraction in general, is what GW Pharma uses for raw BDS for Sativex. Saying that it is might get you shouted down: https://www.icmag.com/ic/showpost.ph...&postcount=155

I stand corrected. A friend of mine showed me the patent that I posted earlier in which CO2 is used as the extraction solvent and he told me it was the process used for Sativex. I will have to ask him some more questions to see why he thinks it is the process for Sativex.

Thanks for the response!

DankTankUSA · May 28, 2012

DankTankUSA said:
I stand corrected. A friend of mine showed me the patent that I posted earlier in which CO2 is used as the extraction solvent and he told me it was the process used for Sativex. I will have to ask him some more questions to see why he thinks it is the process for Sativex.

Ok so I am pretty sure that the patent I posted is the GW Pharma patent on the process used to extract THC and CBN for Sativex. GW Pharma is listed in the patent by name three times. So I think it is safe to say that CO2 is the extraction solvent used in making Sativex.

Lazyman · Jun 22, 2012

Gray Wolf said:
If you have lots of chlorophyll, I infer you are using alcohol to do your RS extraction.

If you freeze the material and chill the alcohol, Ethanol will produce an amber extract in the 3 minute time span Simpson recommends.

If you use Isopropyl, you might freeze and cut your soak time to 20 seconds.

If you already have the ISO oil with chlorophyll in it, you might redissolve it in 190 proof and stick it in the freezer for a couple of days, before straining it through a coffee filter. That will remove some.

If you then stick the alcohol mixture in strong sunlight, it will break down the chlorophyll rapidly into its byproducts within a few hours, which are amber and don't taste green.

Yeah I followed another one of your writeups using a sep funnel and Hexane/saturated saltwater to clean it up, it worked quite well and made some wonderful smooth smoking oil, much lighter in color. The only problem I had was I was cleaning a 9 oz batch of green alcohol oil, and by the time I got that dry (forever) then cleaned it up and redried it (takes even longer to dry hexane) it had been in the oven for over a week at 150*F. I had it lab tested and the potency was only 43% THC< and 12% CBN (indicative of broken-down THC.) Lesson learned, albeit in a slow, painful, expensive way! The 2L seperatory funnel is fun though, was awesome watching hexane strip THC out of alcohol.

I just got into butane, and have a couple big extractors, a big degassing chamber and a wicked 2 stage vacuum pump. Makin wax in bulk, woot! I still have about 40 pounds of trim to process, ack!!!

moresntoil · Jul 13, 2012

epic fail, not my proudest moment.

epic fail, not my proudest moment.

So, im sure some of you will laugh and find this to be quite basic, but i would like to shair this so others may learn from my stupidity.
In the past i have done isomerizations in hexane while refluxing, with great results in fact.

Not having anywhere really to work and lack of time i have tried a much simpler and safer method by just placing everything in a flask and letting it set for a few weeks(or until i get to it) in a dark cool basement of a friend. The isomerization does seem to take place judging by the effect of the oil when vaporized...

The last batch is where everything went south in a matter of 24hrs.
We thought the solution was much more saturated with oil than it usually is so, 2-3 times the amount of sulfuric acid was added......

and.......poof clear hexane with everything GONE! Usually the flask has the garbage at the bottom and the remaining oil still in the hexane.
Im I correct in guessing that you can use too much acid and destroy everything?
the clear hexane does/did have alot of "white pulp" suspended in it, was this wax like you get when making an absolute?

thanks in advance

Gray Wolf · Jul 16, 2012

moresntoil said:
So, im sure some of you will laugh and find this to be quite basic, but i would like to shair this so others may learn from my stupidity.
In the past i have done isomerizations in hexane while refluxing, with great results in fact.

Not having anywhere really to work and lack of time i have tried a much simpler and safer method by just placing everything in a flask and letting it set for a few weeks(or until i get to it) in a dark cool basement of a friend. The isomerization does seem to take place judging by the effect of the oil when vaporized...

The last batch is where everything went south in a matter of 24hrs.
We thought the solution was much more saturated with oil than it usually is so, 2-3 times the amount of sulfuric acid was added......

and.......poof clear hexane with everything GONE! Usually the flask has the garbage at the bottom and the remaining oil still in the hexane.
Im I correct in guessing that you can use too much acid and destroy everything?
the clear hexane does/did have alot of "white pulp" suspended in it, was this wax like you get when making an absolute?

thanks in advance

Good experiment though and only emphasizes the importance of accurate numbers and attention to detail!

We've also found a couple things that don't work well, while poking about, but on the other hand, it is how we've found a bunch of stuff that does.

Ahwooooooooooooooooooooooooooooooo!!!!!!!!!!!!!!!!!1

moresntoil · Jul 17, 2012

thank you for responding GrayWolf,
how right you are. turned out the oil that was left in the hexane was very potent stuff. In fact the amount that was still there was way more that I ever expected by looking at the almost clear solution.
My father always use to complain about what awfull cool-aid my grand father would make when he was a kid. by not measuring the sugar, He'd just "eye it". I should know better! lol

thanks
ps. i was looking at your web site, ITS GREAT!
you guys are sharing so much with so many.

mattkilla420 · Sep 21, 2012

Would this electronic contact cleaner work? I kno its not best Hexane but the only one available on my area. Also do I have to purge it, what does the purging do?
View attachment 183678
Sent from my C771 using Tapatalk 2

Gray Wolf · Sep 22, 2012

moresntoil said:
thank you for responding GrayWolf,
how right you are. turned out the oil that was left in the hexane was very potent stuff. In fact the amount that was still there was way more that I ever expected by looking at the almost clear solution.
My father always use to complain about what awfull cool-aid my grand father would make when he was a kid. by not measuring the sugar, He'd just "eye it". I should know better! lol

thanks
ps. i was looking at your web site, ITS GREAT!
you guys are sharing so much with so many.

Thanks for your good attitude and thoughts bro and good job hanging in there with the hexane extraction!

reefsauce · Jan 7, 2013

Thanks for a very informative thread. And sorry for bumping an old thread up...

I read the thread but was left wondering exactly WHY it is helpful to do an ethanol wash to help purge hexane from the solution?

On the first page GreyWolf mentioned how Ethanol has a higher BP than Hexane.... so to my simple brain it seems like the hexane would boil off at a lower temperature than the ethanol.... but you mention how the higher BP is helpful here. I don't understand... why isn't the hexane easier to purge like butane, because the BP is lower?

Gray Wolf · Jan 8, 2013

Hexane is detectable by taste as low as 30 ppm by some and 130 ppm by the general population. Purging it to those low levels is more difficult than with butane, because of the Van der Waal forces involved with the 50% longer molecule, and the ethanol's bubbling and scrubbing action, help the hexane molecules find the surface and escape.

PhobiaBrixia · Feb 2, 2013

I know this is an old thread but i just need to hear someone on this.
I'm going to attemp an isomerization of industrial hemp leaf oil, which is rich in CBD.
I was thinking of using p-toluenesulfonic acid like in a patent i read but i really need to skip the chromatography separation as for cost.
My idea is extracting big quantities with acetone and winterize it.
Then, after stripping the solvent i would dump hexane and sulfuric acid under stirred reflux for X hours (i need advice on this one), neutralize the solution and then funnel separate with slightly basic water to yeld a smokeable product.

I'm worried about the formation of tar like products i've seen in some isomerization...how i am supposed to get rid of that?

I have pharma grade reagents and a discreet setup, so i'm not one stupid folk who is gonna cover himself in h2so4..

squarepush3r · Jul 13, 2013

ok, this is inspired by Gray Wolf, I tried to clean up some acetone extractions that were pretty cruddy.

This is the first run, its just acetone with some added cyclohexane and normal water, it looks all very dark, I shined a flash light up to show the separation layer to be visible.

This next one is done with more added acetone and normal water, just for experimentation purposes on my curiosity.

This next one is JUST added plan distilled water, just for curiosity, as you can see there are 3 visible layers, I believe the hexane on top, an emulsion ?, and water on bottom.

OK, so now I decided to use some brine, this is brine added after the previous was drained. Notice the brine seems very clear, I don't know what to expect, it didn't seem to drain out any chlorophyll, and the top layer is still pretty dark

At this point I am a bit confused, so I think I'll wait till someone gives me some advice. The brine wash did not seem to get out chlorophyll, but I know the top hexane layer is still pretty contaminated with very dark color and I think lots of chlor.

Shout to to G.Wolf for making this method known.

Waxmasta Flex · Jul 13, 2013

gdub...killin em w knowledge..u go

Gray Wolf · Jul 13, 2013

PhobiaBrixia said:
I know this is an old thread but i just need to hear someone on this.
I'm going to attemp an isomerization of industrial hemp leaf oil, which is rich in CBD.
I was thinking of using p-toluenesulfonic acid like in a patent i read but i really need to skip the chromatography separation as for cost.
My idea is extracting big quantities with acetone and winterize it.
Then, after stripping the solvent i would dump hexane and sulfuric acid under stirred reflux for X hours (i need advice on this one), neutralize the solution and then funnel separate with slightly basic water to yeld a smokeable product.

I'm worried about the formation of tar like products i've seen in some isomerization...how i am supposed to get rid of that?

I have pharma grade reagents and a discreet setup, so i'm not one stupid folk who is gonna cover himself in h2so4..

Technically winterizing is extracting with a non polar solvent and redissolving it a polar solvent to winterize it. Acetone is a polar solvent, so the technique would be limited in effect, but you might try winterizing with something even more polar, like methanol.

We refluxed about an hour and produced the following: The before is on the right, the isomerized on the left, and the pock marks are where samples were taken.

The specs in the before are gnats, which love the stuff if left uncovered.

Gray Wolf · Jul 13, 2013

squarepush3r said:
ok, this is inspired by Gray Wolf, I tried to clean up some acetone extractions that were pretty cruddy.

This is the first run, its just acetone with some added cyclohexane and normal water, it looks all very dark, I shined a flash light up to show the separation layer to be visible.

View attachment 229414

This next one is done with more added acetone and normal water, just for experimentation purposes on my curiosity.
View attachment 229415

This next one is JUST added plan distilled water, just for curiosity, as you can see there are 3 visible layers, I believe the hexane on top, an emulsion ?, and water on bottom.

View attachment 229416
OK, so now I decided to use some brine, this is brine added after the previous was drained. Notice the brine seems very clear, I don't know what to expect, it didn't seem to drain out any chlorophyll, and the top layer is still pretty dark

View attachment 229417

At this point I am a bit confused, so I think I'll wait till someone gives me some advice. The brine wash did not seem to get out chlorophyll, but I know the top hexane layer is still pretty contaminated with very dark color and I think lots of chlor.

Shout to to G.Wolf for making this method known.

Washing won't turn dark oil significantly lighter in color, it just washes out the water solubles and chlorophyll. The chlorophyll isn't really water soluble, but it will wash it away in micelles, because it is polar due to the magnesium atom in its tail.

Darker colors in the depth of solution that you picture, are due to the Beers Lambert effect of looking through that many layers.

Besides the anthro cyanins present, Joe thinks the colors that darken with heat, are caramelized plant sugars, but what ever they are, they will come out using chromotography beads, which strip out the polar elements and pass the non polar solvent and cannabinoids

jump117 · Jul 13, 2013

Gray Wolf said:
.. chromotography beads, which strip out the polar elements and pass the non polar solvent and cannabinoids

Hey Gray Wolf!
Again I am delighted with this photo, excellent color of solution!

It is a pity a little bit that there is no photo "before" for comparison.
How many percent weighed remote "paint"?

Please, you will tell in more detail about this procedure and or properties of the applied materials. It is very interesting!

:thank you:

PS
Such success deserves the separate special detailed illustrated report, much more valid, than a mention of it casually.
It would be very interesting to see photos not only solutions, but also the dried-up extracts "before / after", with the indication of their scales.

squarepush3r · Jul 13, 2013

jump117 said:
Hey Gray Wolf!
Again I am delighted with this photo, excellent color of solution!

It is a pity a little bit that there is no photo "before" for comparison.
How many percent weighed remote "paint"?

Please, you will tell in more detail about this procedure and or properties of the applied materials. It is very interesting!

PS
Such success deserves the separate special detailed illustrated report, much more valid, than a mention of it casually.
It would be very interesting to see photos not only solutions, but also the dried-up extracts "before / after", with the indication of their scales.

The procedure would be similar to Column Chromatography with silica gel. If anyone can get a copy of W.A. Svec, in Chlorophylls, H. Scheer Ed there is a process in there of how to do it. It would be something like this

Extraction of plant pigments
. Extraction of plant pigments from spinach leaves,Spinacia oleraceaL (found inthe local market), were performed by using the already published method [15]. Fresh spinach leaves were firstly depleted from the mid ribs and washed with cold water. The extraction and re-extraction mixtures were methanol and petroleum ether in a 2:1 ratio, and petroleum ether and diethyl ether (1:1), respectively. The methanol removes water from the plant material and the petroleum ether picks up the pigments before they undergo secondary reactions [21]. The diethyl ether increases the pigments solubility in the organic phase. The final extract was a mixture of pigments containing large amounts of various chlorophyll forms, as well as accessory pigments, carotenoids (carotenes and xanthophylls) [21].

Chlorophyll fraction
The chlorophyll fraction – the purified mixture of various chlorophyll forms (e.g. Chl a and Chl b) – was isolated from the pigment extract by using column chromatography with silica gel as the adsorbent (silica gel 60, Merck, 0.063-0.200 mm) and n-hexane/acetone mixture as the eluent [15, 18]. The n-hexane/acetone ratio was changed from the initial 1:0 to final 1:1, to allow
an easier elution of the polar fractions. Chlorophyll fraction was eluted at the eluent composition 1: 0.1 (n-hexane/acetone, respectively), and then transferred in acetone.

jump117 · Jul 13, 2013

I think it is about the ion exchange resins, ion exchangers.

squarepush3r · Jul 13, 2013

jump117 said:
I think it is about the ion exchange resins, ion exchangers.

Ion Chromatography?

jump117 · Jul 13, 2013

Yes, as I understood from earlier report -

Gray Wolf said:
I don't know how these folks are doing it, but Joe has done the ground work for lightening colors using Oregon Medical Growers chromotography beads that looks highly promising.

Most of the more strongly colored material, is also polar, so beads with an ionic charge retain them and pass the non polar cannabinoids in a non polar solvent. The polar elements are then flushed from the beads, using a polar solvent, to regenerate them for reuse.

More on that once OMG gets their packaging completed and are ready to offer their product to the marketplace

Hexane Honey Oil extraction and alchemy

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