No idea if this is kosher, but my intention is only to share what I've gathered... so here goes
Post #12, MidwestHighs: This tek has been around for the better part of the year, I believe FOB extractions was the first to implement it.
If one has a closed loop unit, after you have recycled most of the butane but still have left a decent amount, place your still closed collection vessel into a bucket of dryice, wait until it reads around -40 to -50 on the IR thermometer. After a bit at that temp you can open your collection vessel and either filter threw a buchner funnel or a DIY simple filter setup. Also its best to surround your filtering vessel with dry ice as well so the waxes don't redissolve in the butane as it warms. When using the buchner funnel don't hook your vacuum pump up to it to speed up the process. What one should use is a faucet aspirator with the water flowing outside not down your drain. This will create plenty of vacuum to speed up the filtering in the buchner funnel.
#14 gunnaknow: As an additional note, whether you use butane with alcohol or you use butane alone, the procedure would still be referred to in industry as solvent winterization (as opposed to dry winterization or fractionation). In certain industries, they'll typically use a mixture of solvents at the same time, so a term like single solvent winterization wouldn't really have much use in such industries. However, within the cannabis community, we typically use butane and alcohol in separate stages rather than using a mixture of solvents at the same time. It therefore could make sense to specify if it's a single solvent process or not, as a means to differentiate it from the more typical procedure that we use.
#15 midwesthighs: Ya since it's not like the traditional winterization non polar to polar solvent. Your getting the butane insanly cold so the waxes precipitate out of the solution. Think of a subzero extractor works if cold temperatures keep from dissolving many of these undesirable plant waxes whats to say cold temperatures couldn't make them precipitate out of the butane hash oil solution. I first heard about this about a year ago, but no one was giving up the secret, at the time me and jump brainwashed the idea of how it would work and well kinda figured out how it worked lol. Everyone's calling this dewaxing as to not confuse it with an ethanol winterization. Why so many people love this new method is you hold onto all your yummy lighter
terpenes and flavanoids that would be lost in a traditional ethanol winterization. The results are damn fine, although I haven't been doing much extraction experiments do to current living situations. it'd be nice to see the dewaxing tek preformed then winterize that sample with ethanol to see if almost all or close to all the waxes, lipids and fats are being removed.
#17 gunnaknow: Dewaxing is certainly a suitable term to use, as solvent winterization and solvent fractionation* are methods that can be used in dewaxing. In the vegetable oil industry, they will often remove a considerable amount of saturated fat from the oil, along with the waxes, so although it's often referred to as dewaxed, it's not necessarily just the waxes that have been removed. With cannabis oleoresin, it's predominantly epicuticular wax and much less in the way of fat being removed, so dewaxing is quite an accurate term to use. *solvent fractionation is similar to solvent winterization but the temperature is adjusted more precisely, to separate individual lipid fractions.
#18 gunnaknow: '
it'd be nice to see the dewaxing tek preformed then winterize that sample with ethanol to see if almost all or close to all the waxes, lipids and fats are being removed.' -mwh
I think that that's an important point, midwest. You should in theory be able to precipitate most of the wax, providing that the temperature is low enough, for long enough but once the majority of the wax has precipitated, newly formed wax crystals take longer to grow. If they haven't had time to grow to a sufficient size, it may help to use filter papers with a very small pore size (<3µm). The flow rate would typically be alot slower but the use of a Buchner funnel would largely compensate for that. You could also use glass microfiber filters (Whatman GF/A, etc), to greatly increase the flow rate. I should mention that a relatively low cooling rate results in the formation of larger crystals, which are much easier to filter out. For that reason, it would be a good idea to slowly cool the butane tank to around -20°C in a refrigerator, before placing it in dry ice. Once it has reached it's desired temperature in dry ice, it should ideally be held at this temperature for atleast 5-6 hours, to allow the wax crystals to fully develop. It's often referred to in industry as the maturation time. It sounds like you've done a fair amount of your own research, so this is mainly to help the members here who don't know as much as yourself.
#22 gunnaknow: I can think of a few good reasons why you wouldn't want to use liquid nitrogen. N-Butane and propane have melting points of -138 °C and -188 °C respectively, so unless you're careful to remove the butane tank from the liquid nitrogen at the right point, you could end up freezing the butane solid. Another issue is that liquid nitrogen is so cold that it will cause very rapid cooling, which results in wax crystals that are very small and difficult to filter out. When the solvent is cooled at a slower rate, the level of supersaturation of the solution is limited, which allows the crystals to grow larger. Another issue would be that if you weren't careful to remove the butane tank at the right point, you'd reach the saturation point of the cannabinoids and they too would precipitate out. I hope that this helps.
#23 gunnaknow: If you're concerned that you don't have enough dry ice to give the wax crystals a 5-6 hour maturation period, then you may wish to consider the following procedure. After cooling the collection tank down to the desired temperature, add enough dry ice to a thermos to cool it down to the same temperature and then pour the butane solution from the collection tank into the thermos. The thermos will keep it at this temperature for several hours. The dense layer of butane and CO2 vapor in the head space acts like an insulating plug, so a loose fitting lid will suffice. Just remember to reduce the volume of solution in the collection tank down to an amount that will actually fit in your flask/flasks. I nearly said thermoses but it doesn't quite sound right, lol. It'll be interesting to hear how you all get on with single solvent dewaxing and if you find any additional wax upon winterizing with alcohol.
#24 slimjoint: Hope someone will chime in and provide aittle guidance before i try this. I got a 304 stainless steel beaker which i will blast into it will be sitting in a double boilerin a ethanol dry ice solution. After blasting let it chill for an hour filter out the wax through a buchner , pour the filtered solution onto pyrex and continue usual purge? Are there any additional steps i shoild take? Is it necessary to chill the buchner filter , flask?
After i pour the filtered solution onto the pyrex should the pyrex be warm? Or would extremely cold butane shatter the pyrex plate due to the temperature change?
#25 Green Dot Labs: We do live plant extractions at -150c. No need to dewax anything because plant waxes never dissolve in a solvent that cold.
#27 regisphilburn1: How do you get that cold, liquid N2? Is that in a closed loop? Does THC even dissolve that low? Thats below the melting point (freezing point) of n-butane -138C so its not really making much sense to me. Yes you need to prechill your buchner, no need on final pyrex though, id keep it at outside temp, then move to warm water after a few minutes like usual.
#29 gunnaknow: Pure n-butane would freeze solid at below -140 °C, yes. However, the butane canisters that most of us use contain a mixture of hydrocarbons, including propane, iso-butane and n-butane, among others. The melting/freezing point of such a mixture will be lower than that for pure n-butane. Just as the melting point of water is lowered when it's blended with a miscible solvent with a considerably lower melting point, such as ethanol, glycerine, propylene glycol, etc. However, Green Dot may not necessarily be using butane from canisters.
He's right in the sense that the waxes shouldn't dissolve appreciably in the first place, if the butane is chilled to the desired temperature before and during extraction, rather than afterwards. However, prune has raised a good point regarding the fact that the trichome cuticles contain wax, among other things, which needs to be dissolved or ruptured in order to extract the oleoresin. If the butane is too cold to efficiently dissolve the cuticles, then the only other way for the butane to extract the oleoresin would be for the extreme temperature changes involved to somehow cause the cuticles to rupture. Materials will often experience thermal shock if the temperature change is too drastic, so it's a possibility but it seems unlikely unless he's submerging room temperature material straight into the solvent.
