Bulk Subzero Ethanol Extraction

c03rcion · Nov 21, 2017

WaterFarmFan said:
It definitely sounds dry then if it crumbles. You really just might be going too cold. Start it out of -86C and then place outside the freezer and let the temps rise some to around -50C using a thermocouple to measure.

I have done quite a few ethanol extractions using nothing but trichomes collected from dry ice hash. Most of the trichome matter remains after the ethanol wash, as ethanol only interacts with some of the organic matter that composes the trichome head and stalks.

Ahhhh ok. When I viewed the bud under the microscope, I definitely saw trichome matter--stalks and some heads--but it seemed most heads were gone but some still definitely there
maybe 70% were gone.

Also, I also have a -30 C freezer as well. Maybe I should just keep my ethanol, filters, and tools and bud in the -86C freezer and once I begin the wash process, move the bucket (with ethanol and bud) to the -30 C freezer for the duration of the process. What do you think?

Is there a limit, temperature wise, on the solvent's ability to encapsulate solutes? I think I the -86 C could very well be too cold. I usually see folks perform this method from -50C to 0C. I imagine if the solvent is too cold, there isn't enough kinetic energy in the solvent molecules to effectively solvate compounds.

Thanks for all the feedback!

Gray Wolf · Nov 21, 2017

c03rcion said:
Ahhhh ok. When I viewed the bud under the microscope, I definitely saw trichome matter--stalks and some heads--but it seemed most heads were gone but some still definitely there
maybe 70% were gone.

Also, I also have a -30 C freezer as well. Maybe I should just keep my ethanol, filters, and tools and bud in the -86C freezer and once I begin the wash process, move the bucket (with ethanol and bud) to the -30 C freezer for the duration of the process. What do you think?

Is there a limit, temperature wise, on the solvent's ability to encapsulate solutes? I think I the -86 C could very well be too cold. I usually see folks perform this method from -50C to 0C. I imagine if the solvent is too cold, there isn't enough kinetic energy in the solvent molecules to effectively solvate compounds.

Thanks for all the feedback!

Good job resorting to looking with a microscope!

70% head removal is about the equivalent of the first QWET soak at -18C/0F, at which point you would do a second extraction to glean the balance.

I've never extracted that cold (-86C) before so shooting in the dark somewhat, and have some questions about what components you are extracting at that temperature.

What color and how dark is your low yield concentrate?

c03rcion · Nov 21, 2017

Gray Wolf said:
Good job resorting to looking with a microscope!

70% head removal is about the equivalent of the first QWET soak at -18C/0F, at which point you would do a second extraction to glean the balance.

I've never extracted that cold (-86C) before so shooting in the dark somewhat, and have some questions about what components you are extracting at that temperature.

What color and how dark is your low yield concentrate?

Thanks for the response Gray Wolf. My color and clarity with the low yielding stuff is excellent. Photos attached of my wash solution and final product shatter. I am becoming more convinced that -86C is too cold to do an effective wash as the solvating power of the solvent seems to diminish the colder it gets. I am going to try washing at -30C and see if it helps.

c03rcion · Nov 21, 2017

I have done a few more small test washes and I am still finding trichome heads after washing the bud for about 1 hour in the -30 C freezer. I have tried laying the bud on a paper towel to dry them and rewash, but about 5 minutes into the wash i start pulling some green. I then filter the bud and look at it under the microscope but still find remaining heads.

Any suggestion for the best way to rewash the bud if the desired end product is shatter? How important is it to get the buds dry before rewashing?

Assuming I have 1000 grams of bud @ 20% THC, what would a reasonable expectation for % yield be if the end product is shatter?

Gray Wolf · Nov 21, 2017

c03rcion said:
Thanks for the response Gray Wolf. My color and clarity with the low yielding stuff is excellent. Photos attached of my wash solution and final product shatter. I am becoming more convinced that -86C is too cold to do an effective wash as the solvating power of the solvent seems to diminish the colder it gets. I am going to try washing at -30C and see if it helps.

I would try at -50C. The polarity of ethanol also drops with temperature, so its not as prone to pick chlorophy, and tolerates long soaks.

c03rcion · Nov 22, 2017

Gray Wolf said:
I would try at -50C. The polarity of ethanol also drops with temperature, so its not as prone to pick chlorophy, and tolerates long soaks.

Today I tried two small tests and got around 19% on bud that is in the low 20% for THC-a. I started by staging the bud and ethanol in the -86 C freezer and transferred to the -30 C freezer for the soak, agitating every 10 minutes.

After an hour and a half, the solution looked light yellow but not quite saturated so I tried the -18 C freezer. Maybe 20 minutes later I found the yellow got more intense, almost gold. I started to noticed some green and stopped.

I checked the trichomes after air drying the bud by laying on a paper towel. Some loss of API can be assumed. I washed the bud until most of the stalks appeared furry and minimal trichome heads could be observed.

I anticipate that the remaining trichome heads could be extracted at the expense of some added green pigment to the solution.

Bud was broken apart by hand to sizes not greater than a nickel.

Test 1: 2.6 grams of bud, 19.25% yield
Test 2: 1.6 grams of bud, 17.86% yield

I took a small test bud, along with some ethanol, and put a 50 ml test tube and placed in the -86 C. Even after 4 hours I didn't see green pigment in the solution.

Gray Wolf · Nov 22, 2017

c03rcion said:
Today I tried two small tests and got around 19% on bud that is in the low 20% for THC-a. I started by staging the bud and ethanol in the -86 C freezer and transferred to the -30 C freezer for the soak, agitating every 10 minutes.

After an hour and a half, the solution looked light yellow but not quite saturated so I tried the -18 C freezer. Maybe 20 minutes later I found the yellow got more intense, almost gold. I started to noticed some green and stopped.

I checked the trichomes after air drying the bud by laying on a paper towel. Some loss of API can be assumed. I washed the bud until most of the stalks appeared furry and minimal trichome heads could be observed.

I anticipate that the remaining trichome heads could be extracted at the expense of some added green pigment to the solution.

Bud was broken apart by hand to sizes not greater than a nickel.

Test 1: 2.6 grams of bud, 19.25% yield
Test 2: 1.6 grams of bud, 17.86% yield

I took a small test bud, along with some ethanol, and put a 50 ml test tube and placed in the -86 C. Even after 4 hours I didn't see green pigment in the solution.

Mo betta! The gold you were starting to pull was probably C-40 b-Carotene, and the green clearly C-55 chlorophyll. A good time to stop.

1labs · Feb 11, 2018

May i ask what is the highest yeild of extraction that anyone has seen.
Also what sort of machine and equiptment was used in this process.
Thanks

Gray Wolf · Feb 12, 2018

~25%. Custom built.

1labs · Feb 12, 2018

Hello gray wolf
Im assuming you use flower instead of trim to get those figures correct.

Gray Wolf · Feb 13, 2018

1labs said:
Hello gray wolf
Im assuming you use flower instead of trim to get those figures correct.

Yup! Trim can be anywhere, but typically half or so.

einsteinlady · Feb 13, 2018

Gray Wolf love the design.

After you do bulk subzero extraction, do you/ can you put in a jacketed still (15gal or 55gal)
to reclaim the ethanol and obtain your crude oil?

Also for using a still; whats the largest diameter you would use for a head on a 15gal and also a 55 gal? My thinking is that a larger diameter head = faster distillation time.

Gray Wolf · Feb 14, 2018

einsteinlady said:
Gray Wolf love the design.

After you do bulk subzero extraction, do you/ can you put in a jacketed still (15gal or 55gal)
to reclaim the ethanol and obtain your crude oil?

Also for using a still; whats the largest diameter you would use for a head on a 15gal and also a 55 gal? My thinking is that a larger diameter head = faster distillation time.

Yes, we currently use a simple still, a Extract Craft Turbo vacuum still, a ISO-3 or 4 Isomizer, or a Heidolph rotovape for recovery.

If you wish to keep the extract in carboxylic acid state, vacuum recovery works best.

All things being equal, the greater the surface area, the more surface boiling and with matching condenser, the fastest recovery.

Pressure also affects boiling point and boiling rate.

If you are operating it above one atmosphere (14.7 psi), it is a pressure vessel, so subject to ASME Section VIII.

einsteinlady · Feb 22, 2018

If using a 15 gallon keg;

-What kind of pipe could one use for the column that would still be vacuum rated. Thinking 6" diameter and 36" tall.

-When you say matching condenser, if one used 6'' then condensers I.D. would have to be 6'' too? ... for fastest recovery.

-Attaching vacuum to receiving keg would keep the still at negative pressure. If the vacuum pump failed then positive pressure would form and not be good. A pressure relief valve could be added to the boiling keg. Am I missing something where this would create positive pressure under vacuum????

-Would waterfarms -50degree recirculating cooler be able to keep up with condensing?
For condenser I am thinking a jacketed tube with cold water recirculating through it coupled with a coiled tube inside the condenser also recirculating cold water.

Gray Wolf · Feb 23, 2018

einsteinlady said:
If using a 15 gallon keg;

-What kind of pipe could one use for the column that would still be vacuum rated. Thinking 6" diameter and 36" tall.

-When you say matching condenser, if one used 6'' then condensers I.D. would have to be 6'' too? ... for fastest recovery.

-Attaching vacuum to receiving keg would keep the still at negative pressure. If the vacuum pump failed then positive pressure would form and not be good. A pressure relief valve could be added to the boiling keg. Am I missing something where this would create positive pressure under vacuum????

-Would waterfarms -50degree recirculating cooler be able to keep up with condensing?
For condenser I am thinking a jacketed tube with cold water recirculating through it coupled with a coiled tube inside the condenser also recirculating cold water.

Schedule 5 304SS pipe would work, as would a sanitary coluumn.

6" is a big column!

By matching condenser, I meant one with the same BTU rejection capacity as you are putting in boiling.

What are the specifications on the chiller and how many gallons per minute do you plan to recover?

lawya · Feb 24, 2018

Which do you recommend Gray Wolf? Sub Zero ethanol or BHO?

superglue · Feb 25, 2018

apples? or oranges?
if you are making a pie?
if you are making juice?

fwiw

WaterFarmFan · Feb 25, 2018

superglue said:
apples? or oranges?
if you are making a pie?
if you are making juice?

fwiw

How so? I am curious about the differences. If high quality flowers are used as the source material, what are the apples and oranges?

WaterFarmFan · Feb 25, 2018

Here are my thoughts, which certainly could be wrong as my butane practical experience is nill. Butane has a lower boiling point and better solvent polarity, which makes it easier to extract with, but it is highly explosive and dangerous on a smaller scale without a proper environment. This allows a lower temperature purge (helps keep terpenes) but also picks up more undesirable compounds like waxes, which require further refinement to purify. If that purification is winterization via ethanol, then all the terpenes with boiling points between butane and ethanol will lost during ethanol purge. So, if you are winterizing BHO, why not just extract with alcohol in the first place? I understand that processing low quality trim is much easier to do in bulk via a large closed loop butane system, but volume aside, are there any other benefits to using butane for the smaller craft producer?

Gray Wolf · Feb 25, 2018

lawya said:
Which do you recommend Gray Wolf? Sub Zero ethanol or BHO?

It depends on how much of what are you processing and what do you want to end up with? Might you elaborate?

Bulk Subzero Ethanol Extraction

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