Wiped Film Parameters

thin-film
wfe

#102

We have a CDU and we want it to go faster. Obviously the input feed rate is going to be a big factor. Aside from that we want to make the distillation as effective as possible. For polish run (second pass), we run at 300-400 rpm on the wiper, 170c evaporator face, 130c residual, 70c on the distillate and condenser, and 70c feed input. Feed input is highest 350rpm, we notice worse color any faster. Any ideas would be appreciated. We have experience elsewhere other than wipers. Metering pumps on feed, residue, and distillate output all 300-350. Vac at 7.5 x 10⁻⁴ torr.


#103

“70C feed input” I would turn up the feed temp a bit. I like my feed to preheat to at least 110C- 135C. (Lower range if you can only heat the whole feed flask, 135C if you can heat smaller amounts right before entering still. Notice any vac depth issues at higher feed rate?


#104

Meant rpm


#105

Hello all,

I am running a 6’’ Chinese WFE and have questions about rpm, residence time, etc…

So when running our WFE, i calculate the approximate boiling point of CBD based on our vacuum ( we have it at around 30-50mt). But I’m noticing inconsistencies in our distillate, and I’m guessing it had to do with RPMs and resonance time.

Question being: How does RPM/resonance time affect seperation? I’m guessing that the higher the RPM, the lower the oil bath has to be (to a certain extent), since material is constantly being wiped.

Is there a way to know how fast/slow the rpm should be, and how does it affect the temperature/ evaporation rate?


#106

Usually the blades are designed to force the solution down. That means the faster the RPM the less residence time on the heated portion usually equating into more heat needed. Dial one variable in a time to avoid confusion/frustration in your process.


#107

The less time your material spends on the evaporation surface (usually referred to as “residence time”, although it does go by other names), the hotter the evaporation surface will need to be, or the thinner the film will need to be, or the lower the vacuum will need to be, to achieve evaporation.

so as @710ST suggests, only twiddle one knob at a time :wink:


#108

Hello Brethren,

This is my first time posting, although I’ve been reading for months. I pretty much learned everything (the little) I know so far by reading the threads here. Big ups to Future and the rest of you folks who are sharing so much knowledge and experience.

So after months of reading, I finally set up my spot. I am buying crude to winterize and distill. I am running a 6" chinese WFE. I am degassing in a reactor under vacuum. Below are the settings I am using. Just want to be transparent and share with the others. Not that this is a brilliant setup, or even close.

Winterize:
10:1 alcohol. Freeze for 48 hours. Filter twice through 25 micron then 2.5 micron. Recover in 50L rotovap. My chiller can’t seem to keep up but I can recover about 20L of ethanol every 4 hours.

Degass/decarb:
30L jacketed reactor with Busch MV 0040 pulling vac. Heating jacket with Julabo SE-12. I ramp up temp to 125C over 3 hours then let it sit for two hours at that temp. Agitating with Fusion Fluid lab agitator. The shit that comes out of the pump is GNARLY. I took a whiff and was traumatized for the rest of the night…

Distill:
Given that I am using a chines setup and have not made enough money to update components yet, my vac levels leave a little to be desired. Not sure if I am doing anything wrong, or if its just the price to pay for Chinese equipment, but, at best, vac levels usually hover around 150 mtorr. During my first run I experimented with the evap temp starting at 155C (buddy’s recommendation) going up 5C with each successive pass until I felt that enough of the THC was evaporating. I ended up at 180C on main body (big thanks to Bucky for posting the very thorough SOP above, which has been a major reference point). Using a IR thermometer, I can see that there is a tremendous gradient in heat on the main body, ranging from 179 or so to 157 (that with heater set to 180C). I hope that when I can upgrade to the Julabo on my main rig I will get more consistent temps given the much better circulations speed. The chinese heaters heat well enough, but circulate a snails pace so temperature gradient is very real.
Feed tank set to 90C
THC condenser set to 80C
Terp trap -25C
Cold trap (polyscience IP 100) set to -81
rotation speed between 300-500 rpm. (any advice?)
Feed speed 1L/hr. Supposedly this rig can do 2+L/hr, but I found too much ended up in retentate side, so I slowed it down, perhaps I actually need to slow down my rotors. I thought the faster the speed the better the evap, but after reading above I see that it may in fact push the material down too quickly.
First full run using the protocol I settled on had pretty good results (from visual inspection), no swirls, golden color. Havn’t tested it yet, with the wait times of 2-3 weeks, my sense is that we’ll sell what we have before we get results back. Perhaps naive.

Still not getting the yields I would like. In a 8L run, I ended up with about 4L of distillate (I will definitely rerun to squeeze out every last drop of THC, but looking to speed up the process a little bit) My starting material was good: shatter that didn’t quite make the cut.

A few questions for the generous souls on here:
I started with a little over 20kg of crude/shatter.
-How much should I expect to yield in distillate?
-Should I run evap a bit hotter to get more separation?
-Should I run condenser hotter? Colder?
-How essential is it to get vac levels super low? (After reading bucky’s SOP’s I’m a bit confused, because he said he’s getting super high purity with the vac levels at about 500 mtorr)
-Should I keep feed tank hotter? Originally I had water circulating, but replaced with silicone oil, but I’m scared to heat more than 100C because I’m worried residual water will boil and pressurize jacket, and perhaps blow feed tank. Is that plausible? Or will any vapor go out the tubes with the fluids?
-Any other insights in how to tweak my procedure to get better yields/color/potency? I realize that improving one of those metrics may well decrease the others. Ultimately my goal would be to produce the highest yields possible at or above 85% THC, preferably with one pass through WFE. Possible/plausible?

Also, I would be happy to pay for some consultation time with any of the OG’s on here. Message me if you think it would be a good fit. At present my setup is at my house, so just looking for a phone consultation.

Again, much thanks to everyone sharing their questions and/or knowledge on here. This is the only place I’ve found with legit crowdsourced info. I real gem!

-Tao


#109

Have you had experience on re-running distillate through a WFE? What temps on your evap column and condenser helped?


#110

135/98 evap/cond 50-100mt

Low and slow…