Closed loop recovery times, cooling and heating, vapor assist? Help

Hello everyone, thanks in advance for reading and any help is much appreciated! Im encountering some issues with my recovery times and getting all solvent out of material column in a reasonable time. So I’ll explain the process:

100lb solvent tank
-jacketed
-center coil
Coil condenser
3- 6x48 sleeved material columns
Jacketed collection pot
2-cmep-ol pumps
Coil condenser

I have open sleeve material columns. I fill the sleeve w dry ice and alcohol n pull a vacuum. Then send 70/30 mix from solvent tank, thru a coil that’s in dry ice and alcohol, Into the material column to soak. I’ll leave the solvent to soak the material for 1-1.5 hr . Then dump to collection pot. I’ll then open recovery on collection pot and the recovery on solvent tank, n turn on pump. There is also coil condenser submerged in dry ice n alcohol between pump n solvent tank. So now I’m coming to the issues… it will dump probably about 75% of the Solvent from the material column, then it basically stops. Because the sleeve is so cold, the solvent doesn’t want to come out I’m guessing. And I read about the nitrogen vapor push, but don’t fully understand how to do it properly… So basically I have to wait all day for the column to warm back up and then dump into a different collection pot for a second b grade collection.

Then when recovering, I have a fully jacketed collection pot, n send warm water around it. But the water instantly gets so cold. Idk if my water heater is just a pos or if I need more heaters. Is there one that someone can recommend or the proper way to do it? So basically the recovery is going very slow. I also have a fully jacket solvent tank and the coil down the center, but don’t use them because I don’t have a chiller. Any recommendations on one or the property way to set it up?

And then another issue is when I set up another material column (have a 3 rack set up) and soak it as dump, when I dump, nothing comes out. And I assume this is because the material column is so cold and the collection pot is warm from recovery, so there is a vapor lock?

So basically it takes me all day to run all three columns, when I know there is a way to speed this up. Can anyone help point me in the right direction to getting this system moving better? Thanks!

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Recover from your collection pot until your psi is as close as possible to the psi of the column your dumping since your not doing a vapor push your column isn’t dumping cause it’s so cold.

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You seem to be on a good path. You’ll basically never be a able to dump into a hot pot. I run a cold and hot water bath that I can change back and fourth with valves thru out the day. And yes you probably need a better heater. I run two bucket heaters and it almost never gets cold. Nitro is very easy to run and with a rack mount system I don’t think you’ll ever be happy until you run nitro. If you have any specific questions on it let me know, I recently outfitted mine to run nitro. Its not very expensive. I can dump 4 columns and be fully recovered in maybe 2 hours or less.

Bucket heater
https://www.amazon.com/Precision-Premier-Line-742G-Submersible/dp/B000BDB4UG/ref=sr_1_3?ie=UTF8&qid=1538595948&sr=8-3&keywords=bucket+heater&dpID=41K8PZ5hswL&preST=SX300_QL70&dpSrc=srch

Controller for heater
https://www.amazon.com/Inkbird-Itc-308-Temperature-Controller-Thermostat/dp/B011296704/ref=pd_bxgy_469_2?_encoding=UTF8&pd_rd_i=B011296704&pd_rd_r=f2264d6e-c744-11e8-b5ee-af66c644a3b1&pd_rd_w=XkEmq&pd_rd_wg=ylUUh&pf_rd_i=desktop-dp-sims&pf_rd_m=ATVPDKIKX0DER&pf_rd_p=6725dbd6-9917-451d-beba-16af7874e407&pf_rd_r=WB3H9MKPYAP9Q7Z9KT14&pf_rd_s=desktop-dp-sims&pf_rd_t=40701&psc=1&refRID=WB3H9MKPYAP9Q7Z9KT14

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Also for your tank for now just run ice water thru it via a chest freezer until you buy a chiller. Cheap and effective.

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Handing out all my tricks and secrets I see. Glad it works for ya

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Run a dry ice slurry around a pot with just straight iso in it use an eco 633 pump to pump the alcohol in the jacket and/or the coil. If you do both, use a pump for each, the jacket and the coil. You can pump it down to - 50 or colder once you get the hang of it. That will get your tank cold enough to pull a vac, helping speed up recovery. Use nitro to assist you with pushing your solvent when needed

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Also, try this. When you dump and start recovery, don’t turn on heat to your jacketed pot, let the pump run down the pressure, sucking the solvent from the columns. I know it’s not good for the pumps, but you get em serviced. And it will vac a good amount of the remaining solvent out. When it gets down, shut the valves and begin heating. Try getting another sois vide in your bucket for more heat. What temp do you have it set to? And what pump do you have pumping your water. Look up “eco 396” they are powerful and cheap.

I still owe you for that one. Literally a game changer. Just paying it forward

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I heard about doing the alcohol slurry w the pot of just iso in it to pump around. but I wasn’t sure of what pump was safe to do that with. is that eco 633 safe to use?
and I just had one bucket heater that I don’t think is working to well. would get 80-95 degrees or so. but using it on this new 50 lb collection pot that has a jacket completely covering it its cooling the water very fast. so I just ordered two of those heaters posted above and the controller.

and as far as the nitro push, can u explain? from what I understand u add some in the solvent tank on the vapor port adding up to 90 psi? n then when u opening the liquid port is should push thru n blast out the solvent in the material column? but wouldn’t that just push more liquid in the column? and im unsure how the burping of the nitro works…

what about having a separate solvent tank w a few lb of solvent in it, warming that tank to raise the psi, and then just hooking up the vapor port to column and blasting the solvent out of the column with the high psi solvent? does that work in any comparison to how the nitro works?

The eco pumps are magnetic driven and cold alcohol won’t hurt them. Don’t let ice or dry ice in the pot and they work just great. They can move 20l a min. Use one on the jacket and one one the coil. Once you get her to regulate temp she won’t take too much dry ice.

Nitro assist. My tank has a chiller connected, so she’s always cold and I run passive. So it’s going to be slightly different. But I remove it from my tank before I start recovery. I wouldn’t go that high of pressure. Maybe 40-50 psi. You can murder your cmeps if you jack too much nitro through there. But. If you are cave manning it with the slurry pump. When you dump, you’ll need a hot vapor valve connected. Close liquid liquid line, open vapor and push solvent down. She’ll splatter, continue to recover and shut vapor valve for a moment and let nitro back to the tank. You’ll notice it happening. Open vapor and push any more solvent out. Once nitro is all pushed to your tank shut you pumps off, close recovery on collection and recovery tank with nitro trapped. Bleed off nitro and make sure you don’t let it suck anything in your tank. Stop before then, couple psi stop. I vac it all out of my tank, unless you have the right things in place, don’t do this. Again, still have the Fred Flintstone chillers connected. Open recovery from both and flip on the pump. Now, you may want to turn up your water temp to help feed that pumps desire for pressure, or she’s going to be loud as fuck all day. But the reduced pressure and colder tank should help you recover faster and move that nitro around

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If you use the hot vapor coming from a secondary tank and using it to push your solvent out of your column. You will probably be warming up some solvent far warmer than your desired extract, most likely. Or if your columns are still jacketed, it’ll just turn to a liquid and not give you the desired results

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that was my experience with a warm vapour push…just turned into liquid solvent as soon as it hit the chilled system. Only tried it a couple of times before resorting to N2.

Current team prefers to push with rm temp Propane. I’m not convinced.

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Is a hydrocarbon vapor assist work the same as nitrogen as far as pushing the liquid

I woulden’t be convinced either!

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You’ll need one controller for each of those heaters BTW (pretty sure, I can check later and get back to you)

Every setup is going to be different. I don’t chill my tank, I run it room temp so I’m always sitting at like 50psi enough to fill my columns easily, I only need nitro to push it from the top of the columns and out. However, most people do both. You can def put nitro into your solvent tank as well to push it into the tubes if you are having trouble there as well. As far as burping it, add a line somewhere in your system going outside preferably and just open it with a valve and vent it out. I do mine from a manifold from collection vessel. No need to spend $ on PTFE hoses, just use air compressor hose from home depot.

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Just make sure the hose doesn’t terminate in the parking lot where folks gather to set their meds on fire.

Protocol when I was playing that trick was to do a visual inspection of “outside” before venting through that line.

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At -60C, even a rm temp propane push doesn’t work like pushing with nitrogen.

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Lol, yea thats not a bad idea.

Also, be prepared to spend $500 on buying a “K” size nitrogen tank. Otherwise they will want your social and credit info to “loan” you the tank. Once you buy it, to fill it with HIGH PURITY NITRO (important) is only about $70 and should last you a good amount. Then you just bring it in and swap it. Worth it to call ahead and make sure they have a K size high purity nitro in stock, most places will though.

Buy this regulator from amazon, it cost almost double at praxair. You’ll also need a 1/4 SAE female adapter to use a hose from the regulator to whatever hose you choose (usually 1/4 NPT)

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Ya, I use if instead of nitro because mine is continuous and it wouldn’t work to have to burp nitro. If you have multiple columns running at the same time I go from column to fully recovered column in 25 min . I tried looping 3cmepol’s for a vapor push and it was about 10%as effective as using high psi hydrocarbon

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so u do a push with the high psi hydrocarbon n have good success w it?

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