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Affordable DIY CO2 Extraction???

JYNdustriez

New member
I don't mean to clog the thread but I have not figured out how to edit old posts on here and my thoughts come when they come. Someone mentioned regulating the outflow to keep a constant back pressure while transfering the CO2 in its supercritical state. This is a great idea, with the proper equations for heat and pressure loss a good flow rate could be found in combination with the proper wattage of heat applied. I am studying CO2 depressurization currently to hopefully figure this out.
 

JYNdustriez

New member
I look forward to some input. I don't mind sharing at all. It only makes me nervous because I am showing some ugly in-progress photos of something I wish to one day make a little money out of. I only hope that the primitiveness of my first system, and my willingness to share ANY INFO that I can to help everyone out there with their own DIY set-up does not bite me in the butt. Seriously though, I won't withhold any technique or experience learned from you guys and I won't exaggerate claims. Simply, I want to be a part of the community.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Thanks for sharing bro! A few questions:

How many soak cycles do you typically run and what is the end yield before winterizing?

What are your winterizing losses?

How are you venting off the CO2 after extraction to harvest the oil.
 

JYNdustriez

New member
Sure, before I answer anything though let me spit out a few safety tips.

These cylinders, valves, and gaskets are not designed for constant removal and reattachment.

If you use the supplied, usually buna-n, gaskets on your valve you MUST replace that gasket EVERY time. By the second run all my buna's were trash. Source ptfe o-rings the same size. They work great as far as reusability and sealed just fine for me even though they do not compress like buna.

Use the LEAST possible amount of torque to install the valves, especially since we are repeatedly removing and replacing them. In order to torque valves properly you will need a crow's foot and a torque wrench or some ingenuity and a few tools you already have. I have found that ~40ft-lbs will do but these threads are rated between 50-100ft-lbs. So they can handle more if need be for a complete seal.

Always have the tank valve open when you remove it in order to prevent firing it at your neighbors house.

Clear threads of debris every time before valve re-installation

I think that's it.




How many soak cycles do you typically run and what is the end yield before winterizing?

At least six yoyos of the CO2 back and forth but I like to do eight. From fifty seven grams of medium grade flowertops I collected 9 grams in the end before winterization. That was with pushing a little of ten pounds of CO2 back and forth each time. I never waited for even close to complete transfers. Your weight will certainly be lower than with hydrocarbon solvent.

What are your winterizing losses?

I lost about a gram after thirty six hours in my freezer. I keep saying about because I did not winterize all of my oil together. Some I separated to try different filtration techniques with syringes. Here is a syringe with 1g of winterizing CO2 oil just for fun :) . You may also notice my two lab assistants.



Hydrocarbon solvents grab A LOT more waxes and fats than CO2 does. Every time I winterized I expected the thick layer of in-solubles I always get with hydrocarbon runs. At no point in the pressures I used did CO2 pull out anywhere near as much wax and fat as butane does.

How are you venting off the CO2 after extraction to harvest the oil.

Ok, so for harrvest. The saturated liquid is in the extraction tank with a dip tube. With both tanks connected I push as much liquid as I can to the collection tank without a dip tube. Set the collection tank in the ice water bucket or leave it in room temp to ensure the pressure drops well below supercritical ranges to prevent wastes. Disconnect the collection tank, take it outside, and open the tank valve slightly. The liquid CO2 containing the goodies sits in the bottom and the gas vents away. After the tank is vented reconnect the two together and push more liquid from the extraction tank to vent off. This allows me to push pretty much all of my final saturated contents over to the collection tank.

I was very scared that I was blowing out particulate oil chucks so I fastened a white paper towel over the nozzle and left it to check at the end. It was only moist at the end, no coloration.

After all the saturated liquid is pushed from the extraction tank, and then vented from the collection tank, simply rinse the cylinder with ethanol and pour into a dish or jar. I sourced a brass nipple and cap to make this easier for myself.

That is how I choose to reclaim now.......
 

JYNdustriez

New member
This is how I came up with the eight cycles. For my first run in the 10# cylinder I ensured that I had only 7.35lbs or less of CO2 to give me at least fifty percent headroom. I had never pressurized anything before and did not know how it would behave. With those 7.35lbs at 1300psi I collected the previous .9g cup after ethanol. So 1.22g from 10lbs I could expect using algebra. From experience, a thorough extraction of 57g with hydrocarbons yields me over 10g oil post-winterization. So I though with eight runs ~9.76g. Hoping for a higher purity and therefore expecting a little less weight, I came up with eight runs as a decent number. Especially becuase I wind up transferring a little more than ten pounds of the CO2 each way.
 

JYNdustriez

New member
Apparently not too many care about this topic, but I do. In fact I have been obsessed with it.

Graywolf, I have tested and verified a transfer system to push the co2 as a SC fluid. I have updated my extractor page on my blog with the details that certainly explain enough to DIY. I would post more details here but I am weary of typing.

Also in reference to calculating %volume of liquid co2 in your canisters go by this density for fairly accurate results 0.877 cubic inches per ounce of liquid co2. Got the number here http://www.warpig.com/paintball/technical/gasses/co2dynamics.shtml. Most canisters state a 68% liquid fill volume but this is not based on the density of CO2 which led to my incorrect calculation in the beginning for my 10# cylinder.

Again, I welcome any questions.......................
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Thanks for sharing bro! I'm not obcessed, but keenly interested in the subject.

About what do the CO2 bottles cost, and how many times can you R&R the valve before the threads get marginal?

How are you cleaning the spent plant material out of the tanks afterwards?
 

JYNdustriez

New member
As far as the price, google 20# aluminum co2 tanks with siphon. They must be affordable, or I wouldn't have posted in this forum.

I have removed and replaced the valves in my tank >20 times. So far no aluminum shavings or dust on the brass valve.

From the care manuals of the various manufacturers it truly depends on the torque you use to achieve a gas tight seal. We are not trying to bend the threads upwards only give enough pressure for a cold weld (massive amounts of friction between metal surfaces). Undoubtedly this causes wear in the long run, and again steel tanks outperform aluminum in this area. However, many co2 sources have water condensation, and care for the tanks includes rinsing with warm water. No big deal if you only plan on charging a keg. For our uses not so much. I can not say exactly "after this many runs, the thread will fail". I have not produced any visible damage to the threads and my valves still seat firmly. So I imagine the longevity is pretty good with proper care.

Also, with transferring the co2 as a SC fluid I retained the same weight from my earlier liquid co2 successes but in only five runs. So it must provide some advantage.

None of this is scientific, and full extraction may have been accomplished earlier. However, my goal was to not have to run back and forth to the fill station, nor need some giant reservoir to pump more CO2 after wasting it. CO2 is not expensive, yet it is not cheap enough for an average joe like me to just vent it like crazy. So I can not afford to try a run and vent it at two, three, four, and five cycles. Yet, anyways. Instead I have to over extract every time just to make sure. My accountant (wife) is handy with a pistol and I'm scared :).

Cleaning the tanks is simple. I am going to post a YT tonight on cleaning the tanks, I'll link it here. Always perform a cleaning on a new tank before extraction. Unless you want to see lots of silvery metal show up in your winterization filtration, scary stuff.

All you need is some boiling water, two water pitchers, a funnel, dish soap, and a towel to wrap around the tank.

Boil one pot of water, and fill two pitchers with warm tap water. Grab one pitcher and put a few drops of dish soap inside. Use a funnel and pour the soapy water inside your cylinder. Shake it up and roll it around without spilling to grab all of the contents. Tilt the tank upside down and pour out the liquid. Fill again with the warm water from the second pitcher. Shake, rattle, 'n roll. Pour the liquid out. Now once the pot of water is boiling use the funnel, and carefully(it will shoot boiling water at you if you go to fast) pour the water inside your cylinder. The reason for boiling water is transfer as much heat to the cylinder as possible. This speeds up the drying. If you are concerned, simply use cooler water and wait longer. Wrap your towel around the tank as it will now be very hot then shake, rattle, 'n roll. Pour out the liquid and leave the tank upside down so as much liquid as possible can drain. Then I lay the tank on its side somewhere undisturbed to dry completely, takes about two hours. If you have no time to spare for this then simply conduct all the steps with clean ethanol instead of water and you can continue to extract even with some ethanol left in the bottom of your collection tank. Not the extraction tank however, unless you are making ethanol extracts. Ensure the extraction tank is always dry of any solvent (water,alcohol,etc) used. The one time I cleaned the collection tank with ethanol and left some it nicely left the oils as a puddle on the bottom of the tank after an extraction run. Maybe this is why some claim ethanol as a co-solvent? In any case it did not pose any problem in my mind to have a little in the bottom of the collection tank.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Thanks for filling in some gaps JYN! It answered one cleaning question that I hadn't even gotten around to answering yet.

The unanswered question, is actually how you remove the spent plant material from your tanks after extraction.

Looks like 20# C02 tanks sell at around $105 on Amazon, but it didn't list whether or not it has a dip tube. I will have to check around more.
 

JYNdustriez

New member
I wash my tanks in this manner regardless of the purpose because I am usually not concerned about a little flavor from the previous run.

I simply shake and pour out the spent plant material in my backyard, water it in the grass, and wash out the canister as mentioned.

However, if you wish to thoroughly clean out material from the previous runs, boil some ethanol in the microwave for the final rinse. If there is any oil from the previous run that did not transfer from the extraction cylinder this will remove it along with the plant parts. Isopropyl is much more suited for this task as it is more aggressive but especially because it is cheaper.

I NEVER use iso for winterization or extraction, I am only suggesting it as a cleaning solution to be evaporated.
 

dybert

Active member
Sure, before I answer anything though let me spit out a few safety tips.

These cylinders, valves, and gaskets are not designed for constant removal and reattachment.

If you use the supplied, usually buna-n, gaskets on your valve you MUST replace that gasket EVERY time. By the second run all my buna's were trash. Source ptfe o-rings the same size. They work great as far as reusability and sealed just fine for me even though they do not compress like buna.

Use the LEAST possible amount of torque to install the valves, especially since we are repeatedly removing and replacing them. In order to torque valves properly you will need a crow's foot and a torque wrench or some ingenuity and a few tools you already have. I have found that ~40ft-lbs will do but these threads are rated between 50-100ft-lbs. So they can handle more if need be for a complete seal.

Always have the tank valve open when you remove it in order to prevent firing it at your neighbors house.

Clear threads of debris every time before valve re-installation

I think that's it.




How many soak cycles do you typically run and what is the end yield before winterizing?

At least six yoyos of the CO2 back and forth but I like to do eight. From fifty seven grams of medium grade flowertops I collected 9 grams in the end before winterization. That was with pushing a little of ten pounds of CO2 back and forth each time. I never waited for even close to complete transfers. Your weight will certainly be lower than with hydrocarbon solvent.

What are your winterizing losses?

I lost about a gram after thirty six hours in my freezer. I keep saying about because I did not winterize all of my oil together. Some I separated to try different filtration techniques with syringes. Here is a syringe with 1g of winterizing CO2 oil just for fun :) . You may also notice my two lab assistants.

[URL=http://s7.postimg.org/wgp2lk7tj/IMAG0154.jpg]View Image[/url]

Hydrocarbon solvents grab A LOT more waxes and fats than CO2 does. Every time I winterized I expected the thick layer of in-solubles I always get with hydrocarbon runs. At no point in the pressures I used did CO2 pull out anywhere near as much wax and fat as butane does.

How are you venting off the CO2 after extraction to harvest the oil.

Ok, so for harrvest. The saturated liquid is in the extraction tank with a dip tube. With both tanks connected I push as much liquid as I can to the collection tank without a dip tube. Set the collection tank in the ice water bucket or leave it in room temp to ensure the pressure drops well below supercritical ranges to prevent wastes. Disconnect the collection tank, take it outside, and open the tank valve slightly. The liquid CO2 containing the goodies sits in the bottom and the gas vents away. After the tank is vented reconnect the two together and push more liquid from the extraction tank to vent off. This allows me to push pretty much all of my final saturated contents over to the collection tank.

I was very scared that I was blowing out particulate oil chucks so I fastened a white paper towel over the nozzle and left it to check at the end. It was only moist at the end, no coloration.

After all the saturated liquid is pushed from the extraction tank, and then vented from the collection tank, simply rinse the cylinder with ethanol and pour into a dish or jar. I sourced a brass nipple and cap to make this easier for myself.

That is how I choose to reclaim now.......

This entire thread is a very fascinating read.... I think your lesser wax pulls are due to your protocol, because with our full extractor setup we get LOTS of wax with co2, more so than with butane.

I believe the solvent loading of CO2 is something like 40, which means you need to pump 40 volumes of your solvent through the material, to achieve a full extraction. You may need to do more cycles and it would help to be able to test your material as it goes in, and then again when it comes out. Thats been our best verification tool of our extraction.
 

JYNdustriez

New member
Thank you for chiming in! I have been posting on several forums. This is one of the lesser ones. I have been pretty active on skunkpharm and my own blog. So this technique is a little dated.

I have been getting more wax at my higher pressures but still not as much as with hydrocarbons. Did you use butane under pressure or a glass/steel column? I have butane soaking systems and they extract a lot more wax, and also oil, than the columns. Now I wonder what I am doing that affects this. Thank you for mentioning it. I am extracting ten ounces of plant material tonight at 1600psi/~105F and transferring it for collection at the same pressure. Where did you get the loading capacity numbers from? I based my cycles on the weight I have extracted with a single run of certain weights of liquid co2. Since I am transferring as a gas I assumed that the co2 condensing in the extraction chamber has the same loading capacity as fresh co2 would. Am I wrong? What pressures does your commercial set up extract at?

I will certainly update my blog and these threads with the results and photos over the next few days.

As far as testing, I would love to have this done. However I am not in an area that this is possible. I need to find someone that can have it tested for me.


-JY
 

JYNdustriez

New member
I was thinking also, I have never even researched commercial systems. Nor have I seen one in action. That would be very interesting to me to be able to see. My little system would pee its pants next to yours I'm sure. But they would be designer pants because of the money saved, lol.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
This entire thread is a very fascinating read.... I think your lesser wax pulls are due to your protocol, because with our full extractor setup we get LOTS of wax with co2, more so than with butane.

I believe the solvent loading of CO2 is something like 40, which means you need to pump 40 volumes of your solvent through the material, to achieve a full extraction. You may need to do more cycles and it would help to be able to test your material as it goes in, and then again when it comes out. Thats been our best verification tool of our extraction.

Thanks for sharing bro!

What temperatures and pressures have worked most effectively for ya'll?

Assuming indoor plants, what would you estimate you lose when you winterize?

I qualify it with indoor plants, because we've noted more plant wax in extracts from outdoor plants.
 
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