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Bulk Subzero Ethanol Extraction

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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A couple of previews of things to come when we open our new The Alchemist Resource blog site 11-1-2017.

Here is one system which uses a mag drive pump to circulate -50C ethanol through a column of material and a second that uses either air or nitrogen pressure to transfer the chilled ethanol back and forth.

The ethanol is chilled using dry ice.
 

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Boyd Crowder

Teem MiCr0B35
grabbing the first seat on this one as well
i love that your not laying down after your recent troubles, but ,
continuieng to innovate, mr wolf
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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grabbing the first seat on this one as well
i love that your not laying down after your recent troubles, but ,
continuieng to innovate, mr wolf

Hee, hee, hee, innovation is the fun part and my mechanical and abstract reasoning didn't die with getting out flanked and locked out of SPR, they just sought release elsewhere!!

A kita is a good thing when it drives process evolution to the next level.

It was actually supporting WolfWurx and then Pharmgold that took my attention away from keeping SPR more current and creating new processes and equipment just for fun.

Now that my hut (office) has burned, I (am retired again and) have a better view of the rising moon.

Ya'll will note a number of new designs and improvements when we launch TAR, as well as all new current articles. It will lack some history details, but at this point, those are still available at SPR.

The biggest handicap was having my personal equipment confiscated, thwarting my experimentation, but we've yet to hear from the fat lady on the lawsuit I've filed against James Davies for its return.
 

gaiusmarius

me
Veteran
sorry to hear about your difficulties, haven't been following things too closely recently.
all the best for your new ventures.
 

HG23

Member
I have been working with a Pinnacle Stainless 100L reactor system that is configured just like your second image. It works great and there is no winterization necessary if done cold enough.

The slowest part of the process for me right now is having to remove each bag of material post-extraction and put it in a perforated-basket style centrifuge (Hobart salad spinner) to recover the last bit of ethanol.

You might need some vent ports on your vessels to allow the atmosphere to escape when transferring ethanol around. There is also a small amount to ethanol vapor that escapes from the vent ports during transfer. I currently vent it outside, but it could also be routed to a condenser for collection.

Let me know what you think.
 
Me likey. I've been designing a similar system for winterizing bulk crude. It will utilize a continuous feed centrifuge for filtration and two jacketed fermenters each being chilled by a -120C 30L chiller. I was looking into doing cold ethanol extractions and found that ethanol recovery will be our bottleneck so we try to reduce the amount we need to recover daily by extracting crude with hydrocarbons.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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I have been working with a Pinnacle Stainless 100L reactor system that is configured just like your second image. It works great and there is no winterization necessary if done cold enough.

The slowest part of the process for me right now is having to remove each bag of material post-extraction and put it in a perforated-basket style centrifuge (Hobart salad spinner) to recover the last bit of ethanol.

You might need some vent ports on your vessels to allow the atmosphere to escape when transferring ethanol around. There is also a small amount to ethanol vapor that escapes from the vent ports during transfer. I currently vent it outside, but it could also be routed to a condenser for collection.

Let me know what you think.

Thanks for the heads up, I'll check out the Pinnacle!

The tanks vent through the three way valves. They would have to be vented to the ventillation system, or outside.
 

Old Gold

Active member
We have had no problem pumping as cold as -60C denatured alcohol through our centrifugal magnetic drive pump. It cost roughly $350 from Grainger, and it handles many solvents well (polypropylene). I wanted to test one to see if it would even pump ethanol that is reasonably saturated with cannabinoids and plant extract. I think it will handle pretty well actually...

We also have a jacketed ractor that is over 150 liters. It might help to note that there should be pressure relief valves on there or it must stay vented the whole time (which may be what you said, I wasn't sure). If not, what pressure are you seeing when chilling directly with dry ice?

There is a magnetic stirrer mounted at the bottom, and a 2" drain port. We are going to weld in a filter plate holder to set a bag of material on, as it will sit above the stirrer, and the plate can be removed if needed. Otherwise, we would just stir the plant material directly, which just makes cleanup a lot more time/labor intensive.

We have not run ours yet, but I lean towards a heat exchanger and the mag drive pump instead of direct cooling of solvent like that. Ethanol will likely be stored in a -86C freezer if we run it once a day. Otherwise the heat exchanger is crucial.
 
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Gray Wolf

A Posse ad Esse. From Possibility to realization.
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We have had no problem pumping as cold as -60C denatured alcohol through our centrifugal magnetic drive pump. It cost roughly $350 from Grainger, and it handles many solvents well (polypropylene). I wanted to test one to see if it would even pump ethanol that is reasonably saturated with cannabinoids and plant extract. I think it will handle pretty well actually...

We also have a jacketed ractor that is over 150 liters. It might help to note that there should be pressure relief valves on there or it must stay vented the whole time (which may be what you said, I wasn't sure). If not, what pressure are you seeing when chilling directly with dry ice?

There is a magnetic stirrer mounted at the bottom, and a 2" drain port. We are going to weld in a filter plate holder to set a bag of material on, as it will sit above the stirrer, and the plate can be removed if needed. Otherwise, we would just stir the plant material directly, which just makes cleanup a lot more time/labor intensive.

We have not run ours yet, but I lean towards a heat exchanger and the mag drive pump instead of direct cooling of solvent like that. Ethanol will likely be stored in a -86C freezer if we run it once a day. Otherwise the heat exchanger is crucial.

What horsepower pump are you using brother? I was looking around three hp.

Yeah, a three way valve exhausts in one position and pressurizes in the other. Unless pressurized, the tanks are constantly exhausted.

You are right about requiring a pressure relief, because it is larger than 6" and operating above 15 psi. I'll add one per tank.
 

Gtir

Member
We have had no problem pumping as cold as -60C denatured alcohol through our centrifugal magnetic drive pump. It cost roughly $350 from Grainger, and it handles many solvents well (polypropylene). I wanted to test one to see if it would even pump ethanol that is reasonably saturated with cannabinoids and plant extract. I think it will handle pretty well actually...

We also have a jacketed ractor that is over 150 liters. It might help to note that there should be pressure relief valves on there or it must stay vented the whole time (which may be what you said, I wasn't sure). If not, what pressure are you seeing when chilling directly with dry ice?

There is a magnetic stirrer mounted at the bottom, and a 2" drain port. We are going to weld in a filter plate holder to set a bag of material on, as it will sit above the stirrer, and the plate can be removed if needed. Otherwise, we would just stir the plant material directly, which just makes cleanup a lot more time/labor intensive.

We have not run ours yet, but I lean towards a heat exchanger and the mag drive pump instead of direct cooling of solvent like that. Ethanol will likely be stored in a -86C freezer if we run it once a day. Otherwise the heat exchanger is crucial.


is denatured alcohol ok to use? I would assume methanol and iso would just boil off? but some people have gawked when I mentioned it
 

Gtir

Member
I am currently experimenting with several buckets and Hobart salad spinner, wondering, how many washes can I do on different material, with the same alcohol, my setup looks like this

2 metal water troth buckets nested in each other to create a jacket for dry ice

a chilling coil immersed in a a buket of dry ice

Pour the ethanol through the dry ice coil for on demand cooling

soak the material in ethanol in the dry ice jacketed bucket for 3 minutes

pour through my strainer

throw the wet material in the salad a spinner and spin every last drop out

use the same alcohol and repeat the process with new material

this time when it is in the salad spinner, spray it down with a small amount of fresh ethanol to knock of any concentrate stuck in the material

any flaws in my plan?

https://www.google.com/url?sa=t&rct=j&q=&esrc=s&source=web&cd=1&cad=rja&uact=8&ved=0ahUKEwiGjq_H3_rWAhUNx2MKHVhBAXoQyCkIKjAA&url=https%3A%2F%2Fwww.youtube.com%2Fwatch%3Fv%3D-XP7yflhOtE&usg=AOvVaw3Xe_Y8-pYXGczV_LOjbpgK
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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I am currently experimenting with several buckets and Hobart salad spinner, wondering, how many washes can I do on different material, with the same alcohol, my setup looks like this

2 metal water troth buckets nested in each other to create a jacket for dry ice

a chilling coil immersed in a a buket of dry ice

Pour the ethanol through the dry ice coil for on demand cooling

soak the material in ethanol in the dry ice jacketed bucket for 3 minutes

pour through my strainer

throw the wet material in the salad a spinner and spin every last drop out

use the same alcohol and repeat the process with new material

this time when it is in the salad spinner, spray it down with a small amount of fresh ethanol to knock of any concentrate stuck in the material

any flaws in my plan?

https://www.google.com/url?sa=t&rct=j&q=&esrc=s&source=web&cd=1&cad=rja&uact=8&ved=0ahUKEwiGjq_H3_rWAhUNx2MKHVhBAXoQyCkIKjAA&url=https%3A%2F%2Fwww.youtube.com%2Fwatch%3Fv%3D-XP7yflhOtE&usg=AOvVaw3Xe_Y8-pYXGczV_LOjbpgK

Chilled ethanol is able to hold less solute, and becomes less of a solvent the closer it gets to saturation, which in heaven might be 50%, but is probably closer to 30% at -50C on Earth.

You can check with a 100X microscope and tell how you're doing.

The temperature your ethanol reaches passing through a heat exchanger is a function of surface area, delta temperature difference, and the amount of time involved. An estimate can be readily calculated by converting the R value of the heat exchanger material to K value, which can be done by dividing 1 by R. That will tell you how many BTU's per minute will pass through it per degree difference in delta temperature.

A simpler and arguably more accurate approach if you already have the equipment, would be to run some through first and measure it to see what the temperature actually is.

The goodies we seek are all on the outside of the plant in the form of trichomes, so alcohol that has soaked into the material picks up nothing that we want, and may very well have things we don't want from inside the plant cells. I would suggest keeping that alcohol steam separate until you see what it looks like.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
I have been working with a Pinnacle Stainless 100L reactor system that is configured just like your second image. It works great and there is no winterization necessary if done cold enough.

The slowest part of the process for me right now is having to remove each bag of material post-extraction and put it in a perforated-basket style centrifuge (Hobart salad spinner) to recover the last bit of ethanol.

You might need some vent ports on your vessels to allow the atmosphere to escape when transferring ethanol around. There is also a small amount to ethanol vapor that escapes from the vent ports during transfer. I currently vent it outside, but it could also be routed to a condenser for collection.

Let me know what you think.

Sadly, I couldn't find a picture or description on their site. Do you have a peecture for us'ns to marvel at?
 

Old Gold

Active member
What horsepower pump are you using brother? I was looking around three hp.

Yeah, a three way valve exhausts in one position and pressurizes in the other. Unless pressurized, the tanks are constantly exhausted.

You are right about requiring a pressure relief, because it is larger than 6" and operating above 15 psi. I'll add one per tank.

I somehow got away with 1/4 HP, and it offers 35 ft of head while operating at 14.2 PSI. We are able to push it through two 50 ft cooling coils and two jacketed 12"x30" cylinders simultaneously (inlet at the bottom of jackets). For any seriously large application, surely a 1/2 HP or greater would be minimum.
 

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