Need to increase productivity, advice needed

Help Support and Requests
1

Hey guys, I need help. My lab needs to increase production (more material processed per day) in the next few weeks and I need advice on a few things. I run an Ironfist ex-4 (Haskel ext-420, jacketed collection pot, water heater, condenser coil, solvent tank condenser coil, crappy chiller) , my usual run is a single 5 pound column, which I wash or soak with up to 13 pounds of solvent. Recovery time is usually around 55-75 minutes for a single run but my bosses have requested I “squeeze” as much out of the material as possible so I typically do a second wash of the material and have been averaging run times of 120 minutes in total. I typically can process around 15-20 pounds in a day. Not great, I know, but that would be different if the input material were better.
My questions:

Would a bigger collection pot help? I don’t think it would help me squeeze more runs in the day, as even if I could dump 20 pounds of solvent at single time, it would still take almost as long to recover it, not to mention i’d probably need a bigger solvent tank (our tank holds up to 25 pounds), so that would be 2 fabrications. Any thoughts on this would be helpful or let me know if you agree with my train of thought.

Any chiller recommendations? My dry ice usage is off the charts because my chiller is simply not sufficient. I cool my solvent tank with dry ice while I run and it just eats it up. I am trying to minimize my DI usage. I know there are threads with chiller calculations, but I hate to say, a lot of that stuff is over my head so any advice on chillers or simply pointing me to a good one would be super helpful. Our current chiller is a PolyScience MX07R-20-A11B 7 Liter refrigerated circulator. It simply cannot keep up, it basically acts a thermometer and to keep tank pressure down when I’m not running. I’d like something that could go down to -60c- -80c.

Speaking of dry ice, my bosses want to eliminate the need for it entirely, but I don’t think that is an option. Is there a piece of equipment that could replace the condenser coil? I haven’t seen something like that, but maybe you guys know of something. Just to be specific, a piece of equipment that replaces my dry ice covered coil, cools the solvent and sends it back to the recovery tank? All while working with my recovery pump? I haven’t seen such a thing, but maybe it exists.

I considered the idea of running dual Haskels to speed recovery, but I don’t believe it would be efficient. In such a small single column system, they’d probably be fighting over whatever vapor I produce.

I’ll stop there for now, sorry for the wall of text. My overlords kinda sprung all this on me and want answers, so if anyone could kindly give me some advice I’d really appreciate it. I’m thinking we need to get a completely new extraction system but I’d love to hear your opinions. I’ll be around all day if anyone needs more specifics. Thanks for reading this far and thanks in advance for any help I receive.

2 Likes
2

Pictures of your set up would help.

1 Like
3

IMG_5886
IMG_58863024×4032 1.99 MB

Hope this helpful. I can get more pics if needed.

2 Likes
4

What’s your pressure in collection pot when recovering ?
Is your collection potheated when recovering ?
What’s the diameter of the hose running to the sieves ?

5

The evaporation area I assume is your biggest problem

6

My collection pot pressure never gets very high during recovery, usually no more than 15psi, then dips below that or into negative as solvent is recovered. The diameter of the tubing is 3/8s from the collection pot to the sieve. The collection pot is jacketed and has hot water running through it.

7

How hot is the water when gooing in and how hot coming out?

8

I set my water to about 40c on the way in, it travels through about 12’-15’ of tubing. So i’d imagine it loses some of that heat on the way in. I unfortunately don’t have an output temperature on hand. I could test it right now, but unfortunately i’m not running anything today so I don’t think my output temp would be reflective of an actual run. I’ll try to distill some solvent today and ill get back to you.

9

A larger collection pot will defiantly make recovery faster
I use my collection pot wich stays chilled to receive the blasted butane
With sight glass
I then transfer my cold butane to the next collection pot 12" wich is permanent heated and recovering permanently
With a push off warm vapor butane
The Haskell is at it s limit when your collection is at 2 bar during recovery so plenty of power left

1 Like
10

what is you end product goal? When making shatter I would do 5:1 solvent/material and I would push any solvent out with a hot loop bypass. I don’t have analytics but my yields were excellent.

I would lose about 2pounds of solvent roughly but I would leave my last column up over night and recovery it all back and the sludge that was left was barely a % of my input weight. You should do some tests to see if that second run is worth it

11

Bigger collection pot will speed it up a bit if you’re trying to avoid that second pass

12

My end product goal is usually a nice crumble. With my second wash I get around a 5:1 ratio or sometimes slightly higher. My 5 pound tubes don’t usually hold 5 pounds of material, it averages more around 1800 grams per tube, so around 4 pounds. So here’s a rundown of my extraction: I blast the tube with 13 pounds of solvent (soak/wash), recover until I have enough capacity to wash with another 10 pounds of solvent and recover. Usually takes around 110-120 minutes total. The second wash really helps up the yield, that is for sure.

13

Ohhh you rinse more solvent through during the first run. You should look at getting a larger solvent tank as well as a bigger recovery

What size column is that? How tight do you pack your material? I use a 6x40 column and I could pack 12pounds in there tight

1 Like
14

Yeah, I think the 2 would go hand in hand. The only way for me to actually pull enough solvent out for that kind of capacity would be if I had a larger tank to pull from.

15

One solution is to replace dry ice with liquid nitrogen through its direct addition to extraction ethanol in a VENTED chamber. This is much faster than any cooling method and you can get 100 gallons down to -40 in less than n hour. Warning: this is a potentially dangerous maneuver if you do not know how to operate LN2 canisters, but with the correct SOP it is no problem. I’d be happy to discuss this in more detail over DM and provide both training and an SOP if its appropriate.

1 Like
16

Can LN2 be used for hydrocarbon?

17

Not in a closed system. A custom port will need to be built out of standard triclamp and swagelock parts, and the system will need to be capable of venting pressure constantly during the process.

3 Likes
18

A second solution is to purchase a chiller and ensure that it is sized not using a spreadsheet or fill in formula, but sized through a series of thermodynamic calculations based on your real system. This, long term, is the best option, but up-front is expensive.

2 Likes
19

See you understand thermo dynamics
What is one kg of dry ice in btu or kw approx ?

1 Like
20

if you can run water to waste - use a plate exchanger after your haskel and remove heat of compression with water. if not use a radiator.

2 Likes