Winterization while Blasting?

[BennyHempseed]

Hi All,

Been reading the forum for a while. It has been a great wealth of information through my gardening and processing journey. I've been perfecting a new extraction process over the last few months that involves prolonged reaction times with liquid butane. Without getting to specific about my setup, here's my question:

Is it possible with a 72 micron filter that I am winterizing my reaction during the blast process?

Here's the overview of the procedure: Flowers are added to the extractor and cooled to 32 degrees or colder. Then 2 cans of butane are added to the extractor. The flowers and butane are allowed to mix and react for 45min-1hr at approx. 32 degrees or less. The extractor is gently rolled and mixed several times through the reaction. After the 45min-1hr has elapsed the contents of the extractor are emptied onto the pyrex dish for evaporation. As the contents are released from they extracting chamber they pass through the 72 micron screen. The dish with solvent/essential oils is then brought to evaporate off, eventually scraped and vac purged. And the extractor is emptied.

Here's where my question comes into play. When I'm removing the spent flowers from the extractor I find a layer of light yellow/white 'kief' looking material all caked to the 72 micron filter. My thought initially is that the butane had reached its capacity as a solvent and these were oils/resins washed from the material, but left behind. Initially I began collecting and saving this mystery powder. But at this point I'm pretty convinced it holds little to no active ingredients. My thought now is that these are the same fats and waxes that are removed in the winterization process. Do you think that could be it?

Shout out to Gray Wolf and any other masters of the trade. Would love to hear your input on this.

Photos:
#1 - The caked 72 micron filter at the end of the extraction chamber
#2 - The caked 72 micron filter removed from the extractor
#3 - Mystery powder scraped off the filter
#4 - Closer shot of the powder
#5 - Final product (Pineapple Express), photo doesn't do justice, was clear/light yellow before folded to fit in the NoGoo. Hard like candy now.

Thanks!
Benny Hempseed

 

[BrainChild]

No it's not being winterized (IMO) because you aren't introducing a polar solvent like ethanol to dissolve the non polar waxes & fats. But yes, what you are seeing is the trichome shells and other plant material behind left in the filter. The butane dissolves the oil and leaves most of that plant material behind. I believe what you're seeing is the post extracted resin heads, sans resin.

The extraction teq you describe is interesting...what are you using for extraction chamber if I may? Oil looks great

 

[HashoftheTitans]

Good job! You did what you needed to do. You gave it time to let the waxes fall out and filtered them off. This is considered by some to be winterizing with a single solvent, others call it single solvent dewaxing. Some would say that only adding a second polar solvent blah blah blah... is winterizing. Either way, if your end product doesn't have enough plant waxes to warrant a second solvent to filter off waxes, don't do it. You will be left with a more flavorful and aromatic finished product.

 

[BennyHempseed]

No it's not being winterized (IMO) because you aren't introducing a polar solvent like ethanol to dissolve the non polar waxes & fats. But yes, what you are seeing is the trichome shells and other plant material behind left in the filter. The butane dissolves the oil and leaves most of that plant material behind. I believe what you're seeing is the post extracted resin heads, sans resin.

The extraction teq you describe is interesting...what are you using for extraction chamber if I may? Oil looks great

I think it's definitely waxes of some sort. I don't doubt that there might be a few trich heads in there but I've admittedly smoked a large quantity of the collection before and felt 0 effects. The powder didn't alter the taste of the joint, also didn't enhance any noticeable effects. The extractor is completely custom, all FDA food grade stainless steel. Like I said, I don’t want to go into specifics about it because I’d like to perfect the method before it’s presented to the world.

Good job! You did what you needed to do. You gave it time to let the waxes fall out and filtered them off. This is considered by some to be winterizing with a single solvent, others call it single solvent dewaxing. Some would say that only adding a second polar solvent blah blah blah... is winterizing. Either way, if your end product doesn't have enough plant waxes to warrant a second solvent to filter off waxes, don't do it. You will be left with a more flavorful and aromatic finished product.

Single solvent winterization, eh? I like the sounds of that. The temperature made me think winterization was possible, or partial winterization. I had hoped that it was happening. Winterization, or partial winterization, helps to justify the extra time I’ve given to the extraction. The idea was that an extended reaction time would allow for the liquid butane to react and dissolve the resins on the flowers more efficiently (initially trying to lower the amount of butane used per extraction). But it also occurred to me after that the cold temperatures could be acting to winterize some of the resins and unwanted components as they are caught and pulled through the filter. The characteristics make me think it’s mostly wax product. It doesn’t clump at all. Just remains mostly that powdery kief consistency.


The runs are consistent too. I ran some popcorn Girl Scout flower last night and a quick low heat vac purge produced this shatter consistency oil. Straight form the extractor, hot water bath, scrap and into the vac. Translucent consistency and not sticky at all unless it's warmed.

 

[BennyHempseed]

No one else has any input on this?

 

[BrainChild]

https://www.icmag.com/ic/showthread.php?t=275357

This thread is about single solvent dewaxing, maybe it will help. When I've single solvent dewaxed the waxes came out similar to your pics.

 

[JointOperation]

you know i heard so much about using a buchner funnel.. and just filtering as you spray.. can filter most of the crap out. but havent got a buchner to try yet.. in the process of making a list of shit i need to get to make processing material into bho a easier process until i can afford to make the jump to closed loop.. but as of now.. im saving all the money i make on oil.. for the closed loop.. and vacuum oven.. and a bigger pump ..

right now working with a 3 gallon chamber. and its not bad.. but for production.. LOL.. its not production if u know what i mean.. lol.. im not a big time grower or anything so i dont need anything huge.. but im about quality.. and that will never change.. but honestly... if your going to by a chamber off ebay. and your planning on purging hundred grams at a time.. get a 15 gallon .. so u can do thin and low and slow..

 

[BennyHempseed]

https://www.icmag.com/ic/showthread.php?t=275357

This thread is about single solvent dewaxing, maybe it will help. When I've single solvent dewaxed the waxes came out similar to your pics.

Thanks BrainChild, that post was definitely helpful, as was your input.

you know i heard so much about using a buchner funnel.. and just filtering as you spray.. can filter most of the crap out. but havent got a buchner to try yet.. in the process of making a list of shit i need to get to make processing material into bho a easier process until i can afford to make the jump to closed loop.. but as of now.. im saving all the money i make on oil.. for the closed loop.. and vacuum oven.. and a bigger pump ..

right now working with a 3 gallon chamber. and its not bad.. but for production.. LOL.. its not production if u know what i mean.. lol.. im not a big time grower or anything so i dont need anything huge.. but im about quality.. and that will never change.. but honestly... if your going to by a chamber off ebay. and your planning on purging hundred grams at a time.. get a 15 gallon .. so u can do thin and low and slow..

I think the buchner funnel with liquid butane would be really similar to whats going on with my extraction. I'm going to order some smaller micron screens for my next runs to see if it changes anything. I have a glass pyrex dessicator that fits beautifully in a crockpot. Temperature isn't always accurate but I watched it closely and it does produce quality stuff. Can't beat low heat and a solid vac. Looking to upgrade to a vac oven at some point. Thanks for the input!

 

[Gray Wolf]

Here is the Mk VII conceptual, showing one method of inline dewaxing

 

[BennyHempseed]

Here is the Mk VII conceptual, showing one method of inline dewaxing

Does the Mk VII extraction take place at room temperature?

 

[peter forsbong]

im curious about evap of the ethanol and processes that are used to evap 90% ethanol 10% water??






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Thou shalt seek and respect the opinions of operators, even unto the third helper, for theirs is a wisdom unknown to technicrats.


Wise men learn more from fools, than fools from wise men.

 

[NEGT1]

I'm not sure if 72 micron is best for hydrocarbon extraction or not, it's not the same theory as bubble hash as the trichomes are dissolved.

OP, do you blast at subzero temps?

That will have a fairly large effect on the final product. No it's not technically dewaxing but if you've ever smoked wax'd wax you'll easily notice the buildup of wax and lipids on your nail, blast -0f and the buildup is drastically reduced. Have to believe most of the waxes and lipids are left behind when doing -0f extractions.

 

[Gray Wolf]

Hi All,

Been reading the forum for a while. It has been a great wealth of information through my gardening and processing journey. I've been perfecting a new extraction process over the last few months that involves prolonged reaction times with liquid butane. Without getting to specific about my setup, here's my question:

Is it possible with a 72 micron filter that I am winterizing my reaction during the blast process?

Here's the overview of the procedure: Flowers are added to the extractor and cooled to 32 degrees or colder. Then 2 cans of butane are added to the extractor. The flowers and butane are allowed to mix and react for 45min-1hr at approx. 32 degrees or less. The extractor is gently rolled and mixed several times through the reaction. After the 45min-1hr has elapsed the contents of the extractor are emptied onto the pyrex dish for evaporation. As the contents are released from they extracting chamber they pass through the 72 micron screen. The dish with solvent/essential oils is then brought to evaporate off, eventually scraped and vac purged. And the extractor is emptied.

Here's where my question comes into play. When I'm removing the spent flowers from the extractor I find a layer of light yellow/white 'kief' looking material all caked to the 72 micron filter. My thought initially is that the butane had reached its capacity as a solvent and these were oils/resins washed from the material, but left behind. Initially I began collecting and saving this mystery powder. But at this point I'm pretty convinced it holds little to no active ingredients. My thought now is that these are the same fats and waxes that are removed in the winterization process. Do you think that could be it?

Shout out to Gray Wolf and any other masters of the trade. Would love to hear your input on this.

Photos:
#1 - The caked 72 micron filter at the end of the extraction chamber
#2 - The caked 72 micron filter removed from the extractor
#3 - Mystery powder scraped off the filter
#4 - Closer shot of the powder
#5 - Final product (Pineapple Express), photo doesn't do justice, was clear/light yellow before folded to fit in the NoGoo. Hard like candy now.

Thanks!
Benny Hempseed

Technically winterization is redissolving a non polar extraction, into a polar solvent, and then dropping the temperature low and long enough for the non polar plant waxes to precipitate out, so that they can be removed by filtration.

You have avoided picking up some of those plant waxes by keeping the temperature low, but not so low as to avoid them all with that long a soak.

There are a couple of kinds of wax present, one non polar wax generally coating the plant to keep the water from evaporating away and for UV protection, and another coating the trichomes themselves, that is polar/hydrophylic on the side facing the plant, and non polar/hydrophobic on the side facing the weather.

Nonpolar waxes are easier to remove than slightly polar waxes, when winterizing with a polar solvent.

Time and temperature are somewhat interchangeable.

Alcohol never did like the non polar waxes and if you leave a solution of 190 proof ethanol and BHO sitting on the shelf at ambient temperature long enough, wax will begin to precipitate out with time and first clump and then collect on the bottom of the container.

Dropping the temperature mostly just shortens the time, but also reduces the amount of wax the alcohol can continue to hold in solution. We've winterized in an hour using an alcohol bath and dry ice to produce a -70C bath.

In line dewaxing is a process by which the temperature of the butane is lowered to reduce its ability to hold on to the long heavy plant wax molecules, and if it lowered low enough for long enough before filtering, a high percentage of non polar plant waxes can be removed.

In your case, you are further cooling the butane by releasing its pressure when you discharge it, so while it may start out low in plant wax content, it ostensibly isn't lowered greaty by temperature change at that point.

It may be that sitting for 1 hour has already precipitated out some of your marginally soluble non polar waxes even at 32F.

However, consider that there is more to a trichome than our targeted elements, and taking away those targeted elements leaves some of them hanging in space with their glad faces hanging out.

The waxes covering the trichomes, as well as cellulouse parts like the disc, can easily be washed along and would accumulate on a 72 micron disc, so I suspect what you have are plant fines, mixed with waxes and trichome parts.

We filter at <25 microns nominal, which soon becomes sub micron with pores clogging and the filter cake becoming the filtration media.

 

[Gray Wolf]

im curious about evap of the ethanol and processes that are used to evap 90% ethanol 10% water??

Low heat and simple evaporation.
Accelerated simple evaporation with a fan.
High heat to boil off, with and without recovery.
Vacuum to boil off at low temperature, with and without recovery.

Of the last two, a vacuum oven and a large surface area deep tray works, with a sheet of glass for a bumping spatter shield will get the job done if you aren't in a hurry.

A rotary evaporator is the fastest way I've tried and what I recommend if you are in a hurry and want to keep the heat low.

 

[JointOperation]

its called single solvent dewax.. im not saying u need to spray into the filter while its on.. but u can get the butane cold enough for the waxes and shit to fall out of suspension . so u can filter them.. and not have to introduce another harder to purge solvent..

and yes it can be done. i do it all the time.. without a buchner funnel.. its not getting out as much as winterizing.. but it gets out enough and keeps my smell an taste perfect.

 

[NEGT1]

its called single solvent dewax.. im not saying u need to spray into the filter while its on.. but u can get the butane cold enough for the waxes and shit to fall out of suspension . so u can filter them.. and not have to introduce another harder to purge solvent..

and yes it can be done. i do it all the time.. without a buchner funnel.. its not getting out as much as winterizing.. but it gets out enough and keeps my smell an taste perfect.

How's the shatter stability here?

for anyone really..?

Is a second dewax, or a full winterization needed for a shatter to hold long term @ 70f?

 

[JointOperation]

im getting harder extracts wen i dewax of course.. its the best of both worlds.. im getting like 80-85% the waxes and shit out.. for example. and with a second solvent when i went to try to winterize it with ethanol. i filtered out .8 out of 21 grams..

the smell and taste i lost from the ethanol dewax.. wasnt worth it at all.. and it also changed my color from a nice light orange.. to a dark reddish amber..

so i say.. if you can use dry ice to dewax with just butane.. its your best bet quality wise if you prefer a nice tasty extract.. with pretty close to the same smoothness on the throat and nose.. as a secondary solvent dewaxing..

i think ill stick to the single solvent dewax..

unless for some reason.. or another its needed to be done.. like mold or to filter with a syringe .02 micron filter.. then id just stick to single solvent dewaxing.

also keeping everything as cold as possible the entire way threw and before the extract is super important.. the less you extract the less you need to get out..

 

[NEGT1]

Wait. Are we calling cold extraction, single solvent dewax?

 

[BennyHempseed]

Hi All! Lots of good responses, I regret not checking back on this sooner. I'll detail the process a bit for you. I agree with several responses here, it was waxes falling out of solution during the process.

About the extractor, I ordered a conical shaped stainless steel vessel with triclamp fittings. I noticed when heavily researching extraction (BHO specifically) that exposure to the solvent seemed to be one of the biggest factors in yield (IE. Packing the tube tight to maximize the amount of butane forced into a liquid state so it better saturated the material). My goal was to find a vessel I could put the material in, while keeping the temperature low, to prolong the exposure. The solution I came up with was the extractor I pieced together.

Back to the process/extractor: The vessel can be loaded from one end with the material, then triclamped shut. On the opposite end is a NPT thread triclamp with a needle valve, sealed with Teflon joint tape. Between the valve piece and the vessel is a piece of 15 micron stainless steel screen (upgrade since I was on here last) The whole extractor is about 18" tall and tapers from 5" or so at the one end, to 1.5" at the valve end. The extractor is placed into a 5 gallon bucket, filled with a mix of ice and water.

I fill the extractor with material, allow it to sit in the ice bath for a half-hour to and hour, less if I'm in a rush or trying to do a bunch of runs. Once everything has chilled I fill the extractor from the valve end, it fits about 2 cans + up to 2 oz of material. I wait 10-15 minutes between addition of the first can and second can of solvent. Before I drain the extractor back out I rotate it and shake the contents. You can here the liquid solvent swishing about with the material. After mixing, the contents are drained and you know the process from there - standard boil, vac, etc.

I've tried many variations on the procedure over the years. It was suggested to me to keep the reaction time short, similar to a wash, so I tried that. I've also done prolonged extracts. I think somewhere in-between is the happy medium. Longer seems to be better, because the waxes have more time to fall out of solution. Shorter works too but didn't ever yield anything that was light years better.

I think single solvent dewaxing aptly reflects what's happening. The liquid butane and overall low temps of the extraction process are forcing the waxes out of solution, where they are caught in the filter. It's definitely not fully dewaxed, as I've since winterized with Ethanol and obtained additional waxes from the product. I agreed with JointOperation that winterization removes too much of the terps for me, the extractor does a good job of leaving them intact.

I get a range of oil consistency. I rarely run flowers, as I'm partial to smoking them, so most of my runs are trim. Which speaks to the method I think because I always end up with at least snap-pull consistency. And I've always been able to handle anything I've run at room temp. Sometimes it's fruit rollup consistency, other times it's shatter.

Anyway, I appreciate the comments. I'm happy to elaborate more if needed. I've since moved to a closed loop variation of it. Still involves the original extractor vessel, just added a connection to another vessel contain the solvent and a vessel that the extraction empties into. The whole thing has been an awesome learning experience and I've been lucky enough to enjoy and share quality concentrates with my fellow patients for the last few years. And for less than half the cost of my Vac oven, the extractor and everything I've added/changed has been more than cost effective than anything else I could have bought. I still do personal runs, but I've since turned my focus to breeding.

With that said, if anyone's looking for some genetics I'd be happy to share