Wiped Film Parameters

thin-film
wfe

#1

Hello! I do CO2 extraction and distillation SP and WF. Hoping to discuss some running parameters, I run a 2" Pope system, currently doing 2 passes on winterized, filtered, and de-terp’d material. Seems like we’re getting most of the red out and are getting mid-light amber color. Potency leaves a little to be desired, ~78-88%.

Thoughts?


Dialing in temps on a wfd
Pope 6" thin wipe still and Delta cup15 extractor
Distillation concerns
#2

Have you tried running slightly slower to increase the amount of seporation? What’s in the other 20% of your cromatogram? Are you seeing delta 8 instead of 9?


#3

They’re only testing for cannabinoids, so I’m not actually sure, those percentages are total cannabinoid content.

Edit: The first pass is around 105, 30% rot spd. Second is usually 160, 30% as well.

No delta 8, all 9.


#4

Good, the fact that you have mostly d9 means you aren’t degrading product. I would try to operate the second pass at different perameters and send the samples out for testing. See what samples/ operating conditions give you the best results. Start your run with second pass distlate. varying the speed/ temp every 15 min, collect samples in the middle of each experiment. If it isn’t a theoretal plate issue and your lab tests show some other contaminate you can adapt your sop to remove the unwanted componds.


#5

Right on, was hoping to avoid excessive experimentation, thanks much for the reply though!


#6

How about this? Your 2nd pass has 80% try decreasing the heat to reject an extra 10% . See where that puts you.


#7

If you don’t see an increase in potency from this, it might be that your first pass wasn’t stripped enough and some of the volitiles carry though to the 2nd pass.


#8

Fair enough, I suppose I’ll have to find a happy medium that doesn’t allow too much leftover product in the raffinate. Thanks again.


#9

Whats your internal condenser temp? Running a Pope Hybrid? Have you tried running hot condenser ( greater than 80C )? ( I assume you are good on vacuum. ) Pope hybrids are a bit different than others in that they are a Counter-Current design, which has its advantages , especially when running a hotter internal condenser with complex mixtures.


#10

65C, vac is fine. Have not tried that.

It is not a hybrid, just WF.


#11

What is your internal condenser set to? Have you ever tried running it hotter?

EDIT: Thank you @CollectiveObjective for beating me to it, and with the breakdown of why!


#12

I have some experience running a VTA. Never tried a Pope but I am curious. What is your vacuum depth on each pass? Vacuum levels are more critical for wiped film than for short path, in a sense.

What is your vacuum setup (ie. what kinda hardware)?


#13

Edwards, 2nd pass averages 45 mT.


#14

Edwards 28/30 wet and Agilent dry scroll to the factory Pope cold trap hardpipe. 2nd pass I’ve achieved 25-40 mT on two different Pope systems. The Agilent went deeper; identical setup otherwise. I’ve heard the VTA’s vacuum gets down there…


#15

What do you run your internal condenser at?


#16

70c - 85c, although I’ve heard of people cranking it up to 90c


#17

Oh wow, interesting. I’ll definitely have to play with that more, was too focused on rot speed and dist temps. Many thanks.


#18

That seems to be sufficient for the second pass to me. It’s at the same level of depth as the VTA setup, which uses a diffusion pump to boost depth on the second pass.

What is your evaporator temp and vac level on the 1st pass? If you are getting low levels from your cannabinoid distillate perhaps you need to cut more terpenes out?

Also, what are your feed rates?


#19

Material has the terps taken out via short path.
Vac is around 50 mT on first, 105Cish.
One drop/sec, 30% rot speed.


#20

I also run a 2" Pope and here is what they suggested. Some of the parameters need adjusting depending on your situation but this has been a tremendously helpful starting point.

"Below are some guidelines to get you close enough that you can fine tune your process as necessary. This may not be applicable to other short-path system either. In those cases, there are numerous design differences that can influence optimal processing conditions. Even changes in your feedstock from batch to batch will vary your conditions.

Assuming you do 3 passes, the guidelines are as follows: (This is for the 2” Still, a 4” is about 3x faster rate)

All flows around the same ~250-350 g/hr (some have reported much higher). Temperature and pressure have everything to do with starting concentration, what your goals are, and what you are trying to drive off.

The first pass typically has trace lights, water, etc.) No need for anything g more than weak vacuum (~50-80 Torr), and 80-110C. The condenser only need to be at 25-35. The external condenser you may want to keep cold to capture lighter components.

The second pass is often skipped by folks in your industry. Or the first depending on how you look at it. Here you are looking at mid cut terpenes. Perhaps 1-5 Torr and 120-140C. you will need to optimize this on your end. Condenser at 70C

The last pass is the simplest. Same flow, same condenser temp. The prevailing vapor pressure of the material will be higher than your greatest achievable vacuum. Basically you will want to get as much vac as you can, this should be anywhere from 50-600 mTorr. Start your process here. You will see vacuum getting weaker as you distill and generate more vapors (vapor pressure). This will reach an equilibrium which varies based on your material and how well you did steps 1 and 2. In most cases, you ought to see the vacuum level off between 300-600 mtorr. If you start creeping up to 1 Torr and beyond, step 1 and 2 were fails.

If this is clear as mud or you have any other questions, just let me know.

NOTE: many in your industry have worked this down to 2 steps (combining 1 and 2), and in some cases only one pass through. The trade-off here is purity and color. More passes will give you a compound that is higher in cannabinoid concentration and a much “clearer” look to it. Many have found that the time for more passes hasn’t been worth it (time is money). This would really depend on what the final product is or what your customer is looking for."