Hello all, first time poster. Tried to do my research before asking anything. So I just got an active recovery CLS secondhand-not sure what model, but it’s from TERPP extractors and I’m trying to make sure I have all of my info right before doing a dry run.
I’ve done a lot of research on how to run a closed loop, but everyone I’ve seen has either been top down or bidirectional. It looks like mine is set up to enter the bottom of the extraction chamber. So my question is, do I run it like how I would a top down or is there some special trick with something like that.
Also I’m seeing conflicting reports on whether or not the solvent tank should be iced before the first run or whether its best to have a hot water bath initially for the solvent tank.
My process is going to be
Ice down solvent and extraction column and put collection base in a dry ice bath.
Vac down both extraction collumn and collection base.
Open and fill extraction column with butane. I have a 1 pound column so probably going to run 4 or 5 pounds and let it sit( I have a scale, not sure whether its best to go by weight of solvent or just keep pressure under 70-80psi
Open valve to release solvent mixture into collection base.
Move system so that collection base is in a hot water bath around 95° and put recovery tank and condensing coil in dry ice bath. (Should I vac recovery tank negatively if it is empty?)
Run recovery pump from collection base to condensing coils to recovery tank.
If the solvent is too cold, you won’t have any pressure. This is why some people opt for the warm bath or vapor push. Look into nitrogen assist if you want to run colder.
Don’t bother with dry ice on the collection, it’s not necessary.
Yes, you want to remove ALL atmosphere from the system.
I’d ditch the recovery pump and just run a coil between the collection and solvent tank.
I read that blog or whatever by skunkpharm and it was super helpful. I think I have the IIIA version. I’ll give that other article a read I haven’t heard of greywolf. Thank you!
@graywolf and the other @SkunkyFarmers designed the machine you have…and open sourced the info so we could all have access to effective medicine.
You don’t have to know the history to make hash, but understanding that the guy who designed and wrote the manual for your pipe bomb actually shows up here and answers questions seems worth mentioning…
…and personally, I prefer to have the assigned reading done when the professor shows up to lecture
I appreciate your help! One last question- In my purchase I got 3 20lb butane tanks but only one of them has a liquid and a vapor port, the other two only have one valve. I’m super confused about the functionality of the two tanks with just one port. What can I use the one port tanks for? How do I refill them?
Those are what you take to the store to get more. Although “getting more” maybe non-trivial. You need non-odorized, and most places now require documentation as to why you need it.
It is also possible those are “shipping” tanks, sent from a “refrigerant” supplier. I’m assuming there are still places that will ship “r600”. I’ve never had to go that route.
The tank with two ports is probably a steel hvac industry recovery tank, certainly where I started. Not ideal.
Probably better suited for the task than some of nonsense I’ve seen.
So unless i can find a place to switch it out or fill it, then it’s basically useless? Here’s a pic of my tanks and a pic of my screens after distilling
It looks like you have a Mk III Terpenator with a 6” X 12” lower collection tank? What is your inner column diameter and length?
You noted that was an active system, what does it have for a recovery pump?
A bottom feed terpenator uses approximately three column volumes of LPG.
You first evacuate the whole system to -29.5” Hg, including all the lines, and then flood from the bottom.
If you lay your hand on the tube exiting the top of the column and time how long it takes to flood the column from when you open the valve and when the tube suddenly turns ice cold, you know how long it takes to flow one volume.
You can use that one-volume time to determine how long it takes to flow subsequent volumes.
They are easy to convert to bidirectional flow, in which case you pass two column volumes from the bottom and one rinse volume from the top.
If you wish to soak, then you close the top of the column vent valve when it first overflows and soak for the prescribed period, then open it for the same flood time established by the first flood and again close it for the prescribed soak time. Repeat for the third flood and then close the LPG flood valve and open the dump valve at the base of the column.
You obviously can’t flood more volume than you can hold in the lower tank, so its important to compute your (column versus base size) volumes ahead of time. If you will give me your column size and confirm your collection base size, I’ll run the numbers for you.
The question of heating or cooling your supply tank is a function of head pressure. With straight n-butane, you have no tank head pressure below about 0C and with n-propane mixes, about -41C.
Optimally you would like to flood your column with LPG around -30 to -50C, so as to avoid picking up the heavier non-target molecules above C-22, such as ~C-29 plant waxes, C-40 carotene, and C-55 chlorophyll/pheophytin. It reduces the need for subsequent winterization, with attendant terpene losses.
Unfortunately, you have no head pressure to push the LPG through the column at that temperature, so must either push it through with hot vapor or an inert gas like N2. You can do that by attaching the vapor valve of a second LPG tank that is sitting in hot water, to the vapor valve of your supply tank, or you can attach a N2 bottle at that point.
On the WolfWurx Mk-IV and V systems, we chilled the holding tank to 32F and used a heat exchanger between the supply tank and the column to further drop the temperature of the injected LPG. We chilled the heat exchangers with either a denatured ethanol dry ice bath, or LN2 using a counterflow heat exchanger.
Using 70:30 mix, we had adequate pressure to flood the columns, but they were still set up to use hot vapor assist, which is my preferred crutch, because it doesn’t require subsequent purging, with attendant LPG losses.
An active system will work without a condensing coil between your recovery pump and your supply/recovery tank, but using one allows you to run at lower tank pressures and speeds things up.
On the Mk III we placed the coil in the ice water bath with the supply tank, but the WW Mk IVB/C and VC used an alcohol dry ice bath heat exchanger or a counterflow exchanger using a -15C chiller.
Here is a site with some useful numbers and information on LPG properties:
With regard to your process:
1.0 We packed our columns ahead of time and stored them in the freezer until ready to extract. We chilled our LPG to 0C/32F with an ice bath and set the collection pot in 85F water. Pot heat is to simply replace the refrigeration losses when you boil off the LPG with the recovery pump.
2.0 Vacuum all vessels and all the plumbing to under 10,000 microns or about -29.5”. Analog gauges are not accurate at that level, so consider it -30” Hg on the gauge.
3.0 Start recovery pump and use above bottom flood procedure.
4.0 Use above bottom flood and then dump procedure.
5.0 Collection tank in 85F water. Recovery tank and after pump condensing coil in ice bath. With a pump it is not necessary to use dry ice.
No need to vacuum it out unless it has atmosphere in it. As long as it is only condensable gases, dropping it to subzero temperatures will create a vacuum.
6.0 Yes, the pump hooks to collection tank port and discharges through the condensing coil into the supply/recovery tank.
Oh wow thank you for the response. Yes my lower collection tank is 6" x 12". I’m not sure what the brand or name of the recovery pump, but I’ll attach a photo.
Right off the bat, I’ve done 4 dry runs to distill/clean out the system and I’m noticing some issues.
This isn’t set up as a bidirectional, strictly bottom up. I need to get the valves that will allow me to have a second hose from solvent tank to the top as well as the bottom.
The guage he has is weird and not good. It’s attached to the bottom chamber via several valve extensions and is at the end of a hose, so isn’t directly on the bottom chamber and it reads at 10mmhg at normal levels(I live at right at 5k feet) and when I vac down the system, it reads -5mmhg and my vacuum pump is 12cfm so I’m thinking it’s not my vac pump(also tried a second vac pump to no avail). So I need to get a proper guage for that and I need to get a guage and ball valve for my uppermost connection.
I’m 99% sure I need to change the gaskets as I’m still getting buildup and residue after 4 dry runs.
I’m able to recover all of the butane until it hits the condenser coils. For some reason it does not want to run from the coils to the tank. I have been using regular ice, iso and salt so maybe it’s not getting cold enough
Since I bought this secondhand(got an absolute fuckin steal) I think the mesh gaskets are old and it’s stripping the plastic, I’m ordering new ones before I run it again
New gaskets isn’t a horrible idea. I suggest viton.
If your solvent is actually eating them, then you’re looking at silicone, which has no business in an LPG CLS. I’ve encountered a brand name rig that had 1/2 dozen silicone gaskets scattered throughout when it came in the door (new). So while I doubt you’re dealing with silicone, an applaud “new gaskets” and suggest you up that and get (a supply) of new nuts.
Imo you should also aim to ditch the 6” single pin clamps in favor of the double bolt style. Technically you’d have to do something pretty stupid to get n-butane above the rated pressure for those clamps, but I still suggest changing them.
Unfortunately, if you’re putting the solvent back into the same rusty/gunked tank that it came from, then expecting it to get cleaner makes little sense….were the material column were packed with filter media, you would expect things to improve, but without the ability to clean out the inside of the tank, you’d still never get all the way to clean solvent.
Which is a primary reason folks prefer stainless tanks with removable 6” caps.
Gauges lie. Once you understand how they work, you can appreciate why. Any over-pressurization will permanently deform the Borden tube and give you a gauge that lies.
You can also get hash in there… they make solutions for that. See : Let's see your set up! - #745 by WhereAreTheStones (actually I suggest the whole thread…especially if you’re a visual learner). There are both good and bad examples in there.
Where is that screen located? Below material column, above dump valve?
If what you’re catching is particulate from the tank. Deliberately filtering it before distillation (into a clean tank) would be ideal.
You can probably clean your current tanks (without removing the valves) if you’re determined about it. @SolventDirect_BigM might even be able to offer some tips on appropriate regimen
@GroovyOctopusLabs is correct that servicing that pump before using it is the right move.
