Ethanol wash extraction.

Lucky Luke

Well-Known Member
Looking to do a small Ethanol wash extraction this coming harvest.

What is the easiest and most simple way? Grind dry product ,cover with Ethanol. leave for 1 min. Strain and sit till evaporated?

or?
 

Fadedawg

Well-Known Member
^ any thoughts on this way?

Better to have the trim/popcorn cured?
The extraction is about the same way we do a QWET. We also do a 3 minute wash, but also freeze the material.

Cured is good, totally dry is not, because it makes the material frangible. We leave about 15% water content and freeze the material, as well as subzero the alcohol.
 

gwpharms

Well-Known Member
We fully dessicate the trim or flower and use absolute etoh. (No water allowed) Also it is finely grinded down to maximise surface area and get a complete extraction. You can try cold etoh, it will pull less chlorophyll but you really want to be well below sub zero if you want to get almost zero chlorophyll. Either way you can remove the color and get a red orange yellow or clear oil. Whatever you prefer. I like fine mesh activated carbon for this task. If you go that route learn how to do it right or experience significant oil loss.
 

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BobCajun

Well-Known Member
Interesting about keeping it subzero temp. Hadn't heard that before. To get the cleanest extract though, it might be made with water at about 325-350 f in an enclosed batch reactor. At those temperatures water has similar polarity to alcohol and you actually get higher yields. It's called subcritical water extraction. The pressure from being enclosed keeps it liquid.

I guess you'd have to leach the material with water at normal pressure first so you won't pick up that crud with the pressurized water later, unless you had a way to only have the pressurized heated water ever come in contact with the material. The apparatus is usually constructed so that the extraction vessel and much of the piping is inside an oven of sorts. Temps used are usually 150-200 C, I said 325-350 f earlier, which is about 160-180 C. Obviously water is cheaper and easier to get than other solvents, including CO2. It's also completely non-toxic and environmentally friendly. Just need to use stainless steel pipe for construction. Actually, BHO apparatus may be modifiable, if it's thick enough.

Here's a patent with info on subcritical water.
 
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Lucky Luke

Well-Known Member
Thanks guys for ur input..

Dont forget simple and easy Bob. lol. I dont want to build anythingor muck about to much.

i was going to chill liquid and trim (this should also give the trim more water content??)

Ill call into the local Restaurant supply company during the week and see if i can get some Fryer oil filters at 70 micron.
 

BobCajun

Well-Known Member
I do have a more practical tip, use a French press, a glass one. It'll make it easier. It has a plunger so you can hold the material in when you pour off. This video shows how to put a paper filter in. It's faster than gravity filtering because you apply pressure to push it through.

 
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Lucky Luke

Well-Known Member
I do have a more practical tip, use a French press, a glass one. It'll make it easier. It has a plunger so you can hold the material in when you pour off. This video shows how to put a paper filter in. It's faster than gravity filtering because you apply pressure to push it through.

cool i have one or two of those. The gravity feed is pretty quick if u watched that video i posted though and will probably be faster due to just doing it in one go and not batches.
 

Fadedawg

Well-Known Member
Interesting about keeping it subzero temp. Hadn't heard that before. To get the cleanest extract though, it might be made with water at about 325-350 f in an enclosed batch reactor. At those temperatures water has similar polarity to alcohol and you actually get higher yields. It's called subcritical water extraction. The pressure from being enclosed keeps it liquid.

I guess you'd have to leach the material with water at normal pressure first so you won't pick up that crud with the pressurized water later, unless you had a way to only have the pressurized heated water ever come in contact with the material. The apparatus is usually constructed so that the extraction vessel and much of the piping is inside an oven of sorts. Temps used are usually 150-200 C, I said 325-350 f earlier, which is about 160-180 C. Obviously water is cheaper and easier to get than other solvents, including CO2. It's also completely non-toxic and environmentally friendly. Just need to use stainless steel pipe for construction. Actually, BHO apparatus may be modifiable, if it's thick enough.

Here's a patent with info on subcritical water.
Good score brother BC! Sounds like a fun project worthy of further investigation!

Here is a steam chest table, which shows that at 200C, pressure is only about 420 psi. http://www.turnkeyips.com/assets/steam_temperature_pressure_table.pdf

Attached is a water saturation curve:

My personal experience designing for super heated steam, is limited to a super heater return tube and hydrostatically pressure testing the systems for the US Bicentenial Freedom train 4449 Daylighter restoration in 1976, so would have to refresh my memory to be certain there aren't special rules for super heated steam, but in general ASME Section IX boiler code would require a pressure vessel capable of withstanding 3X the maximum operating pressure and have a pressure relief at about 125% of that pressure.

(Any steam buffs check: http://www.freedomtrain.org/american-freedom-train-home.htm)

1260 psi is not hard to contain in a tube, because the stainless is in tensile, but the end caps become an issue due to deflection, where they attempt to deform into a hemisphere, so the end caps have to be significantly heavier (more beam/depth), to resist it, or start as a hemisphere already.

ASME considers 6" diameter and below piping and above a pressure vessel. Pressure piping rules are easier, because stresses are less, so you will note that SCFE CO2 extraction columns are typically 6".

6" Schedule 40 stainless pipe is rated at 1219 psi, cutting the margin thin, but Schedule 80 is rated for 1913 psi, so would easily work with ANSI flanges and plumbed blind end caps, or ASME dished heads.

http://www.engineeringtoolbox.com/stainless-steel-pipes-pressure-ratings-d_346.html

We used Sprague pneumatic intensifier pumps to pump water at higher pressure, and 420 psi is well within their capabilities on shop air. That is where I would start searching.
 

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Fadedawg

Well-Known Member
i just found this

seems to make it very easy.

Extraction method similar to ours.

Using still or forced air evaporation definitely works, though if the air has much humidity in it, the alcohol will absorb it, which is ostensibly the white cloudy area in front of the spatula in the lower peeeecture. Filtering the dust out of the air is also a good idea.

https://skunkpharmresearch.com/evaporator-chamber/

Not quite as fast, but placing a casserole dish on a 130F heat mat overnight, covered in cheese cloth will also get rid of the alcohol and picks up less water in humid environments.
 

BobCajun

Well-Known Member
This guy used ss pipe for a DIY supercritical CO2 rig, and that must be higher pressure than 150-200 C water. In some states only non flammable solvents can be used, so this would be a good alternative to CO2 for them, depending how well the extract turns out. CO2 extracts aren't that appealing themselves, from what I've read (never tried them), so probably not that hard to improve on.

 
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Lucky Luke

Well-Known Member
Extraction method similar to ours.

Using still or forced air evaporation definitely works, though if the air has much humidity in it, the alcohol will absorb it, which is ostensibly the white cloudy area in front of the spatula in the lower peeeecture. Filtering the dust out of the air is also a good idea.

https://skunkpharmresearch.com/evaporator-chamber/

Not quite as fast, but placing a casserole dish on a 130F heat mat overnight, covered in cheese cloth will also get rid of the alcohol and picks up less water in humid environments.
Great tips, thanks.
 

Lucky Luke

Well-Known Member
OK picked up some filter bags 60-80 microns. (pack of 50 for $20)
and a filter frame to suit. The frames are really cheap at $10.

Can get Ethanol at the local hyrdo shop. I may pop down and get that later today. Im all set up but probably wont do a run until May-June.
 

Fadedawg

Well-Known Member
This guy used ss pipe for a DIY supercritical CO2 rig, and that must be higher pressure than 150-200 C water. In some states only non flammable solvents can be used, so this would be a good alternative to CO2 for them, depending how well the extract turns out. CO2 extracts aren't that appealing themselves, from what I've read (never tried them), so probably not that hard to improve on.

I designed a DIY SCFE CO2 system using standard 4" 304SS Schedule 160 pipe. https://skunkpharmresearch.com/affordable-diy-co2-extraction/

I never built it after experimenting with a loaner passive system and realizing that I couldn't control the pressure temperature curve simply using heat, and that I needed more solvent exchange rate and volume than I had.
 

BobCajun

Well-Known Member
I designed a DIY SCFE CO2 system using standard 4" 304SS Schedule 160 pipe. https://skunkpharmresearch.com/affordable-diy-co2-extraction/

I never built it after experimenting with a loaner passive system and realizing that I couldn't control the pressure temperature curve simply using heat, and that I needed more solvent exchange rate and volume than I had.
Even just copper tubing can take hundreds of psi, steel can take thousands or tens of thousands to burst. Basically any stainless steel pipe system would easily be able to handle superheated water pressure. The question is what would the extract be like? If it's the same as alcohol extract it might not be that great, other than for edibles. Apparently less polar solvents produce the best extracts. I call it Triple Phase CO2 Extraction, entirely new.

I was also thinking about a system using liquid CO2 but with chunks of dry ice still in it. At that point the pressure is only about 5 atmospheres. It's just when it all turns to gas that it gets crazy. So you could make a system out of thick glass so you could visually observe how much ice is left. Just need a safety valve in case it all melts. So you'd have an upper part where you put the dry ice, a middle part with the material and a bottom collector part. The liquid CO2 would drip through as it melts, or get pushed through by it's own pressure. I call it Triple Phase CO2 Extraction. It may be more selective due to lower temp. Can't get much colder than chunks of dry ice right in it.
 
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Fadedawg

Well-Known Member
Even just copper tubing can take hundreds of psi, steel can take thousands or tens of thousands to burst. Basically any stainless steel pipe system would easily be able to handle superheated water pressure. The question is what would the extract be like? If it's the same as alcohol extract it might not be that great, other than for edibles. Apparently less polar solvents produce the best extracts. I call it Triple Phase CO2 Extraction, entirely new.

I was also thinking about a system using liquid CO2 but with chunks of dry ice still in it. At that point the pressure is only about 5 atmospheres. It's just when it all turns to gas that it gets crazy. So you could make a system out of thick glass so you could visually observe how much ice is left. Just need a safety valve in case it all melts. So you'd have an upper part where you put the dry ice, a middle part with the material and a bottom collector part. The liquid CO2 would drip through as it melts, or get pushed through by it's own pressure. I call it Triple Phase CO2 Extraction. It may be more selective due to lower temp. Can't get much colder than chunks of dry ice right in it.
As long as its schedule and size is rated 3X the working pressure as required by ASME. 200C/420 psi maximum operating pressure, would require a rating of 1260 psi at 200C, which as you can see by the chart requires moving to Schedule 80 stainless above 3".

http://www.alascop.com/pdf/cu/water_tubing_1.pdf
http://www.engineeringtoolbox.com/stainless-steel-pipes-pressure-ratings-d_346.html

No clue on what the extract would be like, just trying to present ways to find out for anyone so inclined.

Glass has about the same modulus of elasticity as aluminum, which is about 10 X10-6, so it requires more beam (thickness) than steel, with a modulus of 30 X 10-6.

It is strong in compression, but weak in tension, which a pressurized tube of it would be. It would be easier to put a view port in a steel shell, with a wafer of borosilicate in compression.
 

BobCajun

Well-Known Member
As long as its schedule and size is rated 3X the working pressure as required by ASME. 200C/420 psi maximum operating pressure, would require a rating of 1260 psi at 200C, which as you can see by the chart requires moving to Schedule 80 stainless above 3".

http://www.alascop.com/pdf/cu/water_tubing_1.pdf
http://www.engineeringtoolbox.com/stainless-steel-pipes-pressure-ratings-d_346.html

No clue on what the extract would be like, just trying to present ways to find out for anyone so inclined.

Glass has about the same modulus of elasticity as aluminum, which is about 10 X10-6, so it requires more beam (thickness) than steel, with a modulus of 30 X 10-6.

It is strong in compression, but weak in tension, which a pressurized tube of it would be. It would be easier to put a view port in a steel shell, with a wafer of borosilicate in compression.
Yeah I guess glass would never pass any kind of regulations for a pressure vessel. They would say that it has to be able to take 3x full rt CO2 pressure. There goes my idea for the glass "CO2 Buddy".
 

Fadedawg

Well-Known Member
Yeah I guess glass would never pass any kind of regulations for a pressure vessel. They would say that it has to be able to take 3x full rt CO2 pressure. There goes my idea for the glass "CO2 Buddy".
Glass transfers heat poorly, leading to uneven expansion/contraction, so it also doesn't tolerate thermal shock well either, thus limiting its application around cryogenic liquid air gasses, but CO2's critical pressure of 31.1C/88F at 72.9 atm/1072 psi is still in the range of a compression style view window, so it might work.
 
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