What should I change, bad results!


#1

So I’ve been running distillation for about 3 months and really need some help. My procedure is as follows, I mix my warmed crude at 100f with ethanol at the same temp, sometimes I see immediate seperation after just room temp cooling so I filter through a staged 100 micron cellulose and a 25micron after it. I then place it in dry ice for about 30 minutes and filter through the same 100 and 25 staged filter. After this I freeze to 0 degrees for 12-24 hours and filter through 25 and 8 micron staged filters. The mixture starts black and even after this step the crude is still usually the same dark color. I heat the mixture to about 120f then add about a 1/4 cup of each of summits 3 sizes of carbon powder and a few tablespoons of fullers earth per 150g of resin 1500ml solution. I shake them for roughly 2 minutes then filter through about an inch of celite545 and a 2micron filter. The mixture comes out a deep red color but a very noticable difference from before! I repeat the filtration twice not adding carbon the second time. I move into my rotovap, then after all ethanol is gone i do 4:1 heptsne mix then mix in saline water and seperate 2 times. I then remove heptane and rinse with ethanol. I then activate the crude in my vac oven, no vac, at 200degree for an hour or so. I move the resin directly into my flask all set up ready to go. I run a 5L, with a p6v4 head, 1000ml heads flask, 2000ml for main body, and 1000ml for tails. I generally run about 1200-3000ml of cleaned oil at a time. My procedure goes as follows, I run my condensor at 40c. I start at 60c mantle temp and keep my stirrer at 1000rpm. I start my vac at 15hg and work up to full vac by 100c, my Welch pump holds at around 29.57hg. Usually my mantle over shoots to about 140c during this time and I bump it up slowly about 5c at a time after it drops back to about 120. I usually hit my main body fraction around 215-220 mantle temps but my head temp is around 180-205 and the liquid in the head tends to jump over the top of the vigereux in my head and flows extremely fast and this worries me. I’ve noticed cloudiness before and my distillate is very red. These runs usually take me anywhere from 5-10 hours it seems like start to finish. Please feel free to ask any questions about my process and how I carry it out and any pointers to what i should change I’d very much appreciate it! The material ive been getting to run isn’t of quality and after running about 30lbs of crude into dirty distillate I’m at my witts end please help!


#2

Cloudiness may be that you aren’t winterizing it enough and cold enough, you may want to find a way to winterize it at a colder temp after you filtered it the first time in the freezer. Try winterizing it after first pass. Or are you referring to cloudiness (vapors) in the short path, that might indicate a leak. Red might be a leak in there somewhere. While pulling vac turn the lights in the room low and run s flashlight over the joints and see if you can find the vapor leaks. Before your mantle overshoots, try shutting the heat off so it doesn’t overshoot too much. Is your stir bar full speed by the time you get to full vac. What micron are you running main body at?


#3

Hey man, first thank you for the quick response. So I get a cloudiness in my distillate sometimes, and also get a small amount of smoke during distillation when I get close to the main body. I’m not sure what my micron is but I can check with my regulator, I’m at 29.57hg maybe sways .02. I’ve tried before keeping it on dry ice overnight but it was so slow filtering that cold it seemed like. I use a high temp vac grease from best value, just enough to see a nice clear seal all the way around. My stir bar is consistently at 1000rpm start to finish. I run into the issue of shutting the heat down during main body when the head skyrockets in temp and the distillate is popping like crazy up the head but not overflowing.


#4

I think you need a better vacuum gauge. One that measures micron or mtorr


#5

Ethanol will get thick at colder temps, which will slow down the filtration but it is necessary. You can try winterizing it after first pass, you’ll have less to process, and then run again. During main body, you’ll want to get below 100 micron to be safe. Smoke during the main body, weird. I wonder if you aren’t decarbing it long enough. Also, what pump are you using?


#6

From what I’ve experienced so far, this is what ive seen in relation to head temp and mantle temps. I get dripping going from 60c to 100c(jumps to 140c), my head temp at roughly room temp upto 80c along this time, I collect a heavy cloudy green yellow fraction around 180-200c on the mantle, and the head around 95-120c, then as I move up to 215-225 my head just shoots straight to around 175-190c or higher with a pretty vicious reaction in the head when it starts to overshoot and head goes to around 205c.


#7

I have the Welch 1400.


#8

Also for the regulator/gauge I bought across internationals vac regulator/gauge.


#9

There’s definitely something happening around when your vapor temp jumps up so drastically. Is there a way that you can ramp slower at that point. Insulate your boiling flask with some foil, if you aren’t?


#10

Is your head clogging with oil?


#11

Does the regulator have a micron readout? I think you still need a vacuum guage.


#12

It does have that reading I just hadn’t ever read it during a run. I insulate the flask with foil on the bottom for solid contact and pack around the sides, but considered wrapping up the mantle where the head connects aswell with this insulation rope I have, I hate using it because it never holds tight. I have no issue with my condensor clogging as the distillate seems to be very hot and runs very quickly. I have had the issue before when my condensor was too cold though and used a blow dryer to get her going before it got clogged.


#13

There’s a thread here called “I make terrible distillate” I bet your answer is in there. Almost seems like you are having the same problem. But I also think you should be winterizing it further, as well.


#14

Hmmm i have looked up a welch 1400
IT s cfm is rated at 0.9 that for starters is way way to low on a 5 liter SPD
Try to get your hands on a 20 cfm pump or higher asap secondhand Will do
You really Need a vac gauge in microns asap makes our guidens way more complete even a secondhand hvac gauge Will do we don t have bullseye overhere
I am content with yellow jacket brand
Whenever You see smoke stop all procedures


#15

Ok You have a very complex pre distillation sop sorry to say
So dissolve crude in ethanol
Then make smaller batches for winterization say jugs of 1 gallon A size that your filter (Buchner ?) can handel in 10 min on a 25 micron medium
Put these jugs in dry ice for at least 2 hours to 3 hours
They are on temp once a piece of dry ice When put in the oil /etho doesnt start to boil violantly yust Some action or sinks
Freeze up your filter and filter media
By dropping Some dry ice in 10 minites before starting filtration or in a plastic bag inside your dry ice Cool box
Once every thing is cold start filtration on the 100 mesh size put back in same jug and back in dry ice untill all is filtered
Swap filtermedium to 25 microns and start all over everything has to be cold
Once done You can do your Carbon and fullers earth scubs as You seem fit
I would implement citric acid and bi carbonate in your Brine washes
Check @futere in the pesticide redemiation teck for details
make sure You start with the acid wash
So all is out When You finish ( isomerization)
Then decarb in oven as stated is fine see all small bubbles seize
Then to SPD
The more compounds You get out before SPD the smoother the ride in the SPD less volitilles etc etc
Have a read on your new micron meter If at heads You have 350 microns or less You are good to go
About the new vacuum pump 1x10 4 is the best to get iT has to be 2 stage !!!
And more bigger more better


#16

sounds like your distillation is running really fast, liquid from your boiling flask is most likely creeping up the head. You head temps seem normal, do you reactivate your fullers earth and charcol before adding? I usually heat the powders im going to use to 250c in a rbf and pull a hard vacuum on them. watch for dust getting into your pumps, you need a particulate filter infront of the pump.Are you doing multiple passes on the spd? First pass is extremely hard to get a good smelling and light colored product.


#17

@JohnGrow: looks like you’ve gotten sound advice already :slight_smile:

To paraphrase: Better vacuum and a gauge to prove it.

Then following through the (three now?) community coached SPD threads.


#18

This may be off topic, but why doesn’t anyone utilize bumping stones/boiling chips to stop the aggressive foaming from thca? I have yet to hear about them or see them utilized in this industry and would like to know the reason


#19

that’s what the stir bar is for…

if you’ve got one, it is far more effective than boiling chips.

using boiling chips in your mantle so you can keep going once you’ve degaussed the magnet in there is certainly an option :wink:


#20

:grinning::grinning::grinning::grinning::grinning::grinning: