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Ethanol extraction; Is the short distillation process necessary? After roto vap.

atosvitara

New member
Hi all,


I have been doing research on how to get the best vape pen juice I can get out of my flowers.


Until now it seems the process goes like this: (Really short version)



1- Ethanol bath

2- Filter (#1 lab vacuum filter) (about 2 times)
3- Rotary evaporator
4- Short path distillation? :thinking:


But from all the documentation I have read/watch, only 1 adds short distillation process to get a more pure concentrate. Some use the filter step more times, to get a clearer substance.

The thing is: I'm really ignorant, is all theory for me for now, but I wanted to know before I do my first run, if I should expect lower quality due that I have no distillation equipment.


It seems I have hit a wall, tried to search this info but wanted to check if any of you guys has more info.


Thanks a lot in advance.
 

WaterFarmFan

Active member
Veteran
From my limited experiments with distillate, I would say that there is absolutely no reason at all to do short path when using low temp (-30C - -50C) ethanol extraction and decent or better quality material. If you use older or lower quality trim that generates a crude black looking oil, then distillate purifies the oil significantly, but, and I truly think this is a VERY BIG BUT, in addition to terpenes, distillate removes and alters the lesser cannabinoids that also play a decent part in overall effect (IMHO for effect - THC > Terpenes > Lesser Cannabiniods). I think this is why distillate is often flat.

So, you absolutely do not need short path equipment to make vape oil, and if you use good quality flowers to extract with, short path will actually make your vape oil worse. You are much better off to focus your energy on doing the coldest extraction possible (with dry ice) to ensure the highest quality product for vaping. Hope this helps.

WFF
 

dybert

Active member
From my limited experiments with distillate, I would say that there is absolutely no reason at all to do short path when using low temp (-30C - -50C) ethanol extraction and decent or better quality material. If you use older or lower quality trim that generates a crude black looking oil, then distillate purifies the oil significantly, but, I am truly think this is a VERY BIG BUT, in addition to terpenes, distillate removes and alters the lesser cannabinoids that also play a decent part in overall effect (IMHO for effect - THC > Terpenes > Lesser Cannabiniods). I think this is why distillate is often flat.

So, you absolutely do not need short path equipment to make vape oil, and if you use good quality flowers to extract with, short path will actually make your vape oil worse. You are much better off to focus your energy on doing the coldest extraction possible (with dry ice) to ensure the highest quality product for vaping. Hope this helps.

WFF

Most distillation does not split the minor cannabinoids from THC or CBD.
 

WaterFarmFan

Active member
Veteran
Most distillation does not split the minor cannabinoids from THC or CBD.

Is this because the distillation cow is allowed collect a larger range of boiling points? I found the below interesting:
Here is a nifty list that I scored off ICMag, posted by Spurr, who used https://cannabis-med.org/data/pdf/2001-03-04-7.pdf as his information source:

?-9-tetrahydrocannabinol (THC) Boiling point: 157C / 315 degree Fahrenheit ( Merck 200C @0.02). Properties: Euphoriant, Analgesic, Antiinflammatory, Antioxidant, Antiemetic

Cannabidiol (CBD) Boiling point: 160-180*C / 320-356 degree Fahrenheit Properties: Anxiolytic, Analgesic, Antipsychotic, Antiinflammatory, Antioxidant, Antispasmodic

Cannabinol (CBN) Boiling point: 185*C / 365 degree Fahrenheit Properties: Oxidation, breakdown, product, Sedative, Antibiotic

Cannabichromene (CBC) Boiling point: 220*C / 428 degree Fahrenheit Properties: Antiinflammatory, Antibiotic, Antifungal

Cannabigerol (CBG) Boiling point: MP52 Properties: Antiinflammatory, Antibiotic, Antifungal

?-8-tetrahydrocannabinol (?-8-THC) Boiling point: 175-178*C / 347-352.4 degree Fahrenheit Properties: Resembles ?-9-THC, Less psychoactive, More stable Antiemetic

Tetrahydrocannabivarin (THCV) Boiling point: < 220*C / <428 degree Fahrenheit Properties: Analgesic, Euphoriant

Terpenoid essential oils, their boiling points, and properties

ß-myrcene Boiling point: 166-168*C / 330.8-334.4 degree Fahrenheit Properties: Analgesic. Antiinflammatory, Antibiotic, Antimutagenic

ß-caryophyllene Boiling point: 119*C / 246.2 degree Fahrenheit Properties: Antiinflammatory, Cytoprotective (gastric mucosa), Antimalarial

d-limonene Boiling point: 177*C / 350.6 degree Fahrenheit Properties: Cannabinoid agonist?, Immune potentiator, Antidepressant, Antimutagenic

linalool Boiling point: 198*C / 388.4 degree Fahrenheit Properties: Sedative, Antidepressant, Anxiolytic, Immune potentiator

pulegone Boiling point: 224*C / 435.2 degree Fahrenheit Properties: Memory booster?, AChE inhibitor, Sedative, Antipyretic

1,8-cineole (eucalyptol) Boiling point: 176*C / 348.8 degree Fahrenheit Properties: AChE inhibitor, Increases cerebral, blood flow, Stimulant, Antibiotic, Antiviral, Antiinflammatory, Antinociceptive

a-pinene Boiling point: 156*C / 312.8 degree Fahrenheit Properties: Antiinflammatory, Bronchodilator, Stimulant, Antibiotic, Antineoplastic, AChE inhibitor

a-terpineol Boiling point: 217-218*C / 422.6-424.4 degree Fahrenheit Properties: Sedative, Antibiotic, AChE inhibitor, Antioxidant, Antimalarial

terpineol-4-ol Boiling point: 209*C / 408.2 degree Fahrenheit Properties: AChE inhibitor. Antibiotic

p-cymene Boiling point: 177*C / 350.6 degree Fahrenheit Properties: Antibiotic, Anticandidal, AChE inhibitor

Flavonoid and phytosterol components, their boiling points, and properties

apigenin Boiling point: 178*C / 352.4 degree Fahrenheit Properties: Anxiolytic, Antiinflammatory, Estrogenic

quercetin Boiling point: 250*C / 482 degree Fahrenheit Properties: Antioxidant, Antimutagenic, Antiviral, Antineoplastic

cannflavin A Boiling point: 182*C / 359.6 degree Fahrenheit Properties: COX inhibitor, LO inhibitor

ß-sitosterol Boiling point: 134*C / 273.2 degree Fahrenheit Properties: Antiinflammatory, 5-a-reductase, inhibitor
 

dybert

Active member
Is this because the distillation cow is allowed collect a larger range of boiling points? I found the below interesting:

The problem with all these boiling point charts is that they never give pressure. I've seen 10 different charts with 10 wildly different "boiling points" for THC, for example.
 

atosvitara

New member
Thanks a lot!


This is makes sense. I will start to experiment with the coldest temps I can.


Any though on the filter step? I can't seem to find any directions on the temperature for filtering.




From my limited experiments with distillate, I would say that there is absolutely no reason at all to do short path when using low temp (-30C - -50C) ethanol extraction and decent or better quality material. If you use older or lower quality trim that generates a crude black looking oil, then distillate purifies the oil significantly, but, and I truly think this is a VERY BIG BUT, in addition to terpenes, distillate removes and alters the lesser cannabinoids that also play a decent part in overall effect (IMHO for effect - THC > Terpenes > Lesser Cannabiniods). I think this is why distillate is often flat.

So, you absolutely do not need short path equipment to make vape oil, and if you use good quality flowers to extract with, short path will actually make your vape oil worse. You are much better off to focus your energy on doing the coldest extraction possible (with dry ice) to ensure the highest quality product for vaping. Hope this helps.

WFF
 

WaterFarmFan

Active member
Veteran
Any though on the filter step? I can't seem to find any directions on the temperature for filtering.

Not much out there on -50C filtering. Here is one of my previous posts on the subject:

https://www.icmag.com/ic/showpost.php?p=8201105&postcount=26

Basically, I started using 1 liter glass buchner with Whatman #1 filter paper and some radiant barrier material to make a sleeve and lid around funnel. Dry ice would go around glass outside funnel in sleeve and keep the funnel -50C during the 20-30 minute filtering process.

This worked great, but the 1 liter funnel size only made smaller runs possible, which led to me to my current solution of a custom stainless steel buchner funnel:

https://www.icmag.com/ic/showthread.php?t=352154&page=3

The trick to maximizing yield (and keeping the filter cake in -40C to -50C range) is explained in first link but involves the continued addition of virgin -50C etoh until all extract laden alcohol has been collected. Depending on the dryness and consistency (flower vs trim), a decent percentage of alcohol will remain wetted on the material. The concept is that fresh -50C etoh will replace the extract laden etoh that wets material during the vacuum filter process.

Hope this helps.

WFF
 

DemonTrich

Active member
Veteran
Toss in some.dry ice to your etoh, and try and keep at -50c. And use 200 proof etoh, not that store bought garbage.
I use a welch wobl bac pump, 600/2000ml buchner fuller with fritted disc, 200 grit aluminum oxide, and a deep freeze.
 

atosvitara

New member
Damn that looks impressive, congratulations.



Not much out there on -50C filtering. Here is one of my previous posts on the subject:

https://www.icmag.com/ic/showpost.php?p=8201105&postcount=26

Basically, I started using 1 liter glass buchner with Whatman #1 filter paper and some radiant barrier material to make a sleeve and lid around funnel. Dry ice would go around glass outside funnel in sleeve and keep the funnel -50C during the 20-30 minute filtering process.

This worked great, but the 1 liter funnel size only made smaller runs possible, which led to me to my current solution of a custom stainless steel buchner funnel:

https://www.icmag.com/ic/showthread.php?t=352154&page=3

The trick to maximizing yield (and keeping the filter cake in -40C to -50C range) is explained in first link but involves the continued addition of virgin -50C etoh until all extract laden alcohol has been collected. Depending on the dryness and consistency (flower vs trim), a decent percentage of alcohol will remain wetted on the material. The concept is that fresh -50C etoh will replace the extract laden etoh that wets material during the vacuum filter process.

Hope this helps.

WFF
 

atosvitara

New member
Toss in some.dry ice to your etoh, and try and keep at -50c. And use 200 proof etoh, not that store bought garbage.
I use a welch wobl bac pump, 600/2000ml buchner fuller with fritted disc, 200 grit aluminum oxide, and a deep freeze.


Thanks a lot, I am having a lot of trouble keeping all in -50c, it is way harder than I though.



How long do you keep the material with the ethanol before filtering?
 

WaterFarmFan

Active member
Veteran
Thanks a lot, I am having a lot of trouble keeping all in -50c, it is way harder than I though.

How long do you keep the material with the ethanol before filtering?

It definitely takes some time to bring room temperature etoh and plant material down to -50C. I plan about 3 hours myself. You also really need to insulate your coolers. I use tons of this:

https://www.homedepot.com/p/Reflectix-48-in-x-25-ft-Double-Reflective-Insulation-BP48025/100052556

https://www.homedepot.com/p/Reflectix-2-in-x-30-ft-Reflective-Foil-Tape-FT210/100318556

I have a very thick (+2") wall foam cooler and then put 3-4 layers of insulation on bottom and all walls. Lid has multiple layers of insulation taped to bottom as well. If you are using a large traditional hard shell cooler, then with the insulation material make a box in box.

Thick wall glass, like the Everclear bottles, will have better heat transfer (and cool faster) than thinner ones. I also highly recommend using a stainless container to pre-cool your material. You want your flower/trim material as close to -50C as possible as well.

I have seen dry ice added directly to plant material and inside etoh to cool faster, but I am personally against this practice. First is the sanitariness of the actual dry ice. Some is certainly better than others, but I have seen them use shovels to weigh out bulk quantities and the grocery store variety always seems to have a bit of an odor. Another one is if you immediately vacuum distill etoh to bulk remove, then you can get very explosive bumping that sends concentrate past traps and into receiver, as the dry ice (pure c02) carbonates the alcohol. That being said, I have used dry ice directly a few times when plant material was not cold enough, and I was worried about water soluble pickup.

As for soaking times, if my material and etoh are both in the -40C to -50C range, I have let it soak for up to an hour. My filtering process takes another 30 minutes, so these have to be added together. Usually it is about 30 minute soak with filtering becomes an hour. Once I add -50c ethanol and material together, I add dry ice to cold trap and stainless filter sleeves, which gives these about a half hour to cool down prior to filtering, so it works out quite nice.

I would guess that I use about 15-20 pounds of dry ice, including slab that stainless material container sits on, for this part of the process, but I will also re-use (from etoh glass cooler) this same dry ice for my bulk etoh removal as well.
 

atosvitara

New member
It definitely takes some time to bring room temperature etoh and plant material down to -50C. I plan about 3 hours myself. You also really need to insulate your coolers. I use tons of this:

https://www.homedepot.com/p/Reflectix-48-in-x-25-ft-Double-Reflective-Insulation-BP48025/100052556

https://www.homedepot.com/p/Reflectix-2-in-x-30-ft-Reflective-Foil-Tape-FT210/100318556

I have a very thick (+2") wall foam cooler and then put 3-4 layers of insulation on bottom and all walls. Lid has multiple layers of insulation taped to bottom as well. If you are using a large traditional hard shell cooler, then with the insulation material make a box in box.

Thick wall glass, like the Everclear bottles, will have better heat transfer (and cool faster) than thinner ones. I also highly recommend using a stainless container to pre-cool your material. You want your flower/trim material as close to -50C as possible as well.

I have seen dry ice added directly to plant material and inside etoh to cool faster, but I am personally against this practice. First is the sanitariness of the actual dry ice. Some is certainly better than others, but I have seen them use shovels to weigh out bulk quantities and the grocery store variety always seems to have a bit of an odor. Another one is if you immediately vacuum distill etoh to bulk remove, then you can get very explosive bumping that sends concentrate past traps and into receiver, as the dry ice (pure c02) carbonates the alcohol. That being said, I have used dry ice directly a few times when plant material was not cold enough, and I was worried about water soluble pickup.

As for soaking times, if my material and etoh are both in the -40C to -50C range, I have let it soak for up to an hour. My filtering process takes another 30 minutes, so these have to be added together. Usually it is about 30 minute soak with filtering becomes an hour. Once I add -50c ethanol and material together, I add dry ice to cold trap and stainless filter sleeves, which gives these about a half hour to cool down prior to filtering, so it works out quite nice.

I would guess that I use about 15-20 pounds of dry ice, including slab that stainless material container sits on, for this part of the process, but I will also re-use (from etoh glass cooler) this same dry ice for my bulk etoh removal as well.




I was reading your Stainless Buchner funnel post.
Any chance you have a video or pictures of it working? :shucks:


I get the general idea. This pops in my mind.


1- Why put the material with the etho on the funnel and not do a pre filter with a 220 micro filter? just to get rid of the big chunks.


2- Closing it with a lid, the whole setup, doesn't the dryice generate a lot of gas rising the inside pressure? Well I guess that helps with the vaccum and filter speed.


3- You talk about a cold trap, what do you use it for? To keep the vacuum pump safe?



Hope you have pictures of this setup!!
 

WaterFarmFan

Active member
Veteran
I was reading your Stainless Buchner funnel post.
Any chance you have a video or pictures of it working? :shucks:

I get the general idea. This pops in my mind.

1- Why put the material with the etho on the funnel and not do a pre filter with a 220 micro filter? just to get rid of the big chunks.

2- Closing it with a lid, the whole setup, doesn't the dryice generate a lot of gas rising the inside pressure? Well I guess that helps with the vaccum and filter speed.

3- You talk about a cold trap, what do you use it for? To keep the vacuum pump safe?

Hope you have pictures of this setup!!

I have been quite busy, but I intend to make a long thread with many photos of the process.

1.) I pulverize (smash the shit out of) all material as it is freezing in stainless container. so there are no chunks at all. I think this helps to get max extraction. Vacuum filtering helps to suck much of the ethanol from material, but it is the continued addition of fresh -50C that replaces ethanol soaked on plant material, again to get max extraction. I also press the material in funnel to form a dense filter cake, which will clog any filter with enough material, including a 220 filter. My current filter stack consists of 25 micron pre-filter (Whatman #4) and a 2.5 micron (Whatman #5) final stage.

That was the long answer, but short is that if leave material in big chucks and pre-filter like that, you will not get as much yield. You could immediately re-freeze material and potentially do a second soak to get more yield, but the chances for picking up water soluble nasties increases greatly. That is more of quick wash (QWET) that uses short soak and filter times but also warmer ethanol. If you keep that etoh and material below -30C (-50C best), then long soak times don't matter.

2.) The cold gas actually helps cool everything quicker. If you want to be safe, you could drill a few very small holes, with a bit of simple tape to act as an emergency pressure relief, but it should be fine either way, as very few things are completely air tight.

3.) Yep, cold trap keeps the vacuum pump from blowing up and starting a fire. It is a pure safety device. I do not have a rotovap, but instead use 24/40 vacuum distillation glassware. This cold trap prevents etoh vapor from distillation from reaching pump:

https://www.ebay.com/itm/1-5-Gallon-2qt-tank-Dry-Ice-Cold-Trap/282344169244

If you are bulk removing ethanol in another way, like rotovap or still, then you really only (if you want to be super safe) need something like this to prevent an emergency overflow of your receiver:

https://www.ebay.com/itm/30-200MM-Glass-Ice-Cold-Trap-Absorber-Apparatus-Lab-Glassware/151299171035

If you are just looking for an efficient way to make clean ethanol extract, then the filtering setup below is pretty straight forward:

https://www.ebay.com/itm/1000ml-24-40-Glass-Buchner-Funnel-With-90mm-Pore-plate/231771734870

https://www.ebay.com/itm/2000ml-24-...1-neck-2Litre-Lab-Boiling-Vessel/331236947757

https://www.ebay.com/itm/Whatman-10...m-Dia-Grade-1-100-pk-PN-1001-090/252899296376
 
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