Unique THCA/THC extraction and purification Tek.

[Smokin Moose]

This was posted at my home site at TY and thought I would share it here.

 

Posted by Pflover 25/6/09

 

Here is a patent on a very unique THC extraction and purification process that relies on extraction THCacid using an acid/base extraction technique. It's intriguing if nothing else. I've tried a simplified version of the process out and altho not that great of a yield off dried bud it did work and seem to produce a very pure product. The yield made me wonder if it might be more effective with wet bud. Interestingly it yields both a high grade "honey oil" (which the patent actually suggests is tossed) and this purified THCA/THC.

 

Production of .DELTA. 9 tetrahydrocannabinol

 

ABSTRACT:

.DELTA.9 THC acid is obtained from plant material and extracted into an aqueous solvent under conditions of pH control. The acid is converted to a salt and the salt extracted into a polar solvent, yielding acid of high purity. The .DELTA.9 THC acid is then converted to .DELTA.9 THC which is further purified and combined with a carrier for pharmaceutical use.

 

In the patent:

 

Bud is ground to fine homogeneous flour consistency.

 

This is then extracted with an alkane or mix of alkane solvents. Methane, butane, hexane, and octane are all alkane solvents. The inventors consider hexane to be the best they tested. This is done at room temp.

 

The solvent is filtered of plant matter and the plant matter is discarded.

 

The THCacid (THCA) is extracted from the alkane solvent into a second saline aqueous solvent with ph of 12.7-13.2. This is achieved by taking saline (sodium chloride solution) and adjusting the ph to 13 with sodium hydroxide. It is possible to make a ph as low as 12 but best purity is achieved between 12.7-13.2. Ph above this can start to degrade the THC and below this will allow more CBD and other impurities to migrate to the aqueous solvent. The sodium hydroxide reacts with the THCA converting it to THCA Sodium salt which is more soluble in the polar aqueous solvent than in the non-polar hexane. (The sodium chloride is used to inhibit an emulsion layer from forming between the two solvents.)

 

The two solvents are separated and here the inventors throw out the THC containing hexane.

 

The remaining aqueous solution containing the THCA salt is then combined with DIPE (diisopropyl ether) at which point the THCA salt preferentially migrates into the DIPE. The inventors suggest other ethers could be used here but that the extraction in this step would not be as complete as with DIPE as the salt seems significantly more soluble in DIPE than water but not so much with other ethers. It is a shame DIPE is not easy to get and is dangerous to store. The use of DIPE here also further purifies the THCA. The DIPE is then washed with a small amount of clean base/saline solution.

 

The DIPE is then acidified to a ph of less than 3 using dilute hydrochloric acid.

 

The acidified DIPE is then filtered through diatomaceous earth to remove any remaining plant matter. The acidification is crucial before this step because the THCA salt will not pass through the filter.

 

The DIPE is then refluxed for 10 hours with a 22% sodium hydroxide solution to decarboxylate the THC, preferably in a nitrogen atmosphere.

 

The THC containing DIPE is then filtered through activated charcoal and evaporated to yield 95-99% pure THC.

 

They suggest several ways of refining it further.

 

What I did:

Powdered bud in coffee grinder making sure to get every bit back out that I could.

 

This was extracted at room temp for 30min in to Turpenoid , a mix of long chain alkanes and filtered.

 

This was mixed thoroughly with twice the volume of calcium hydroxide-saturated saline solution, ph ~12.5, for 1hr.

 

The solvent layers were separated and the Turpenoid layer was evaporated to yield honey oil.

 

The aqueous layer was adjusted to a ph of 2-2.5 using citric acid.

 

A small amount of coleman naphtha (~1/5th the volume of Turpenoid used) was then added and the to solvents were thoroughly shaken together for 20 min. The naphtha was pulled off the top. More naphtha was added, shaken and separated 2 more times.

 

All three runs of naphtha were then combined and evaporated. The last bit of residue was removed with the help of a double boiler.

 

This resulted in a yield which was part tan oil and part what appeared to be THCA salt.

 

This was cured over night.

 

When smoked the high was sharp and distinctive when compared to either the source material (tyson) or the honey oil and distinctly more potent than the honey oil drop per drop.

 

This Tek could potentially be used as a step in the BHO making process since butane is an alkane. With dried bud however the yield is not particularly worth the effort (3g==>3-6 hits "pure" plus 15-20 hits honey oil). It might be more worth it with wet bud or leaf or with already kiffed bud.

 

It would also probably improve yield to follow their recipe exactly but I did the best I could under the circumstances.

 

Source: http://www.treatingyourself.com/vbulletin/...ead.php?t=37647

[luciddreaming]

I thought THC by itself was a bad high? Or does this maybe extract CBD also?

[Radic]

yep dat a delta9 THC extract

very unstable

sooooooo

smoke the whole lot there and then

100m oil dema call it

cause it never travells more than 100m from the maker

irey guidance

[Radic]

seen

i have tried this too

and just like pflover

i simplified the process to suite i

starting from BHO

the only way that i know of to desolve delta9 thc into water is to lower the PH to 4.8

i have used vinega and lemmon juce as PH down

worked a treat

timing is crucial

you need to work fast

the lower PH you go the faster thc desolves into the acidic water

add the BHO and gently stir it till you can see little cloudy, creamy white swerls as the delta9 thc desolves

after some stiring time the little coluds will stop happening

then strain

and

pour the water into a clean container

baseify the water as it comes back up to ph7

the delta9 THC will drop out of the water and sink to the bottom

yes little ceamy white cystals

let it settle

pour the water off

true a coffie filter

squeese it dry

and smoke it there and then

seen

the bigest problem is that delta9 thc is very unstable and needs to be keeped in an, air tight, light tight (dark container) in the fridge

or elce you might as well smoke it all right there and then

you wont get much quanity either

the more pure you go

the smaller the yeild will be

as for the stone

strictly ireyness

but

as a standard and for eaze of storage

i prefier bho

i like the cbd-thc-cbn ballance

delta9 thc by its self is not as good as bho

this is all strictly personal prefferance

others may not agree

imo

bho rulez

i dont bother going past there for irey oils