Terp Trommel!

[Gray Wolf]

Who ever it was, was babbling on the SPR site, tossing out utter BS, inappropriate insults, and threats to shore up a seemingly saging ego, so was asked to play nice once and then tossed.

Even if he had a valid patent, which he doesn't, it would only give him the right to spend all his money defending it, and doesn't cover the first amendment rights of others.

As RB notes, it appears to be just someones need for more love and drama in their lives and went nowhere.

 

[SkyHighLer]

The earliest history of BHO,

https://www.icmag.com/ic/showthread.php?p=7670567#post7670567

 

[superglue]

nope, indra = john ≠bubbleman

Ricky´s Quote "A nice bit of theater by bubbleman to generate drama, nothing else." relates to a HashChurch episode in which Indra showed up.

It´s funny because the cornerstone of extraction tek in the US relies basically on patent infringement.

thanks for the clarification
it seemed a bit out of character for bubbleman but weirder shit seems to happen

 

[Breakover]

Very interesting, I just got a Pope still and if I feed at the recommended rate I don't seem to fully distill the material in a single pass. I realize this is an old post and you may have a totally different process now but can you tell me more about why you feed so slowly and what happens if you don't?

Sure!

You are correct I have tweaked my method since then.

What was happening when I ran too fast was either streaking or severe yield loss. I was also not degassing enough. Solved the degassing issue and it got better.

Running hotter and faster now, figured out that a hot condenser is a friend indeed. Still not at 1l/hr, but much closer than before.

New parameters are 145-160c and 95 c. Let vacuum settle in where it will, no adjustment of vacuum necessary.

 

[HG23]

Good to see you posting again Breakover. Thanks for the new info.

Can you elaborate on how you solved the degassing issue?

I have a WF still on the way and am interested in how you clean and prep crude oil prior to distillation. I'm planning on winterizing, carbon scrubbing and filtering over silica, reducing the solution in a rotovap, then decarbing and loading into the still. What do you think?

 

[Breakover]

That's more than we do at the moment.

We winterize, then after the ethanol is recovered, I crank the rotovap bath to 95 and 100 mbar and degas it for an hour or so, depending on size.

Then I load the feed flask on the wfe, and degas it further. I usually start my drip once the vac drops below 200 mTorr.

The big difference seemed to be the degas run in the rotovap. Feed flask degassing only takes 15-20 minutes now.

 

[HG23]

Interesting. I remember the Pope guy telling me it was really important to get as much ethanol out as possible pre distillation. By feed flask degassing do you just mean heating it up in the feed flask until it stops bubbling before starting to feed the still? What temp do run it at to degas? Do you back it down before you start to feed?

This also fits with what easystephen posted recently about rotovaps vs cylindrical methods of evaporation. At a certain size cylinders have an evaporative surface area advantage but, their methods of use usually involve short residence time and are expensive. In contrast, you can hold material in a rotovap as long as you need in order to degas as you describe.

So do you always keep the condenser set at 95C and run the evap hotter or colder between 145-160C depending on the quality/clarity of the starting material? Do you do a deep cut and a light cut or do you keep the parameters the same and just keep putting the material back in the feed flask for successive runs until it's refined enough?

Sorry for all the questions, my Pope is set to get here this week and I haven't had time to go out there to WI for the training. I would rather get info first hand here from actual operators anyway. Any other tips you or easystephen can lay down would be much appreciated while I'm getting everything setup.

If you haven't seen it, check out Summit Research's video about their winterizing/dewaxing filter aid. It really clued me in as to how carbon filtering and using a silica filter bed works. It seems like it would be extremely useful and could potentially save time/cost.

 

[Breakover]

I'm still playing with the parameters, but that evap temp range consistently gets the color and potency we're after in one pass. No need to re run. I will run hotter and faster with 'cleaner' starting material to minimize waste. Have to run dirtier stuff slower and cooler to avoid streaking.

I probably need to step up my filtering process, I'll check out summit's vid, thanks!

And yes, on the degas question. We remove as much alcohol, water, and terps as we can before distillation. I try to get the feed flask about 120-140c and just wait for the bubbles to slow and stop. I don't always wait until it's completely stopped, just when it's slowed to an occasional bubble or two.

 

[Chunkypigs]

....
And yes, on the degas question. We remove as much alcohol, water, and terps as we can before distillation. I try to get the feed flask about 120-140c and just wait for the bubbles to slow and stop. I don't always wait until it's completely stopped, just when it's slowed to an occasional bubble or two.

have you figured out a way to extract the terps into a nice product like we are starting to see on the market while you are degassing or even before you extract the cannabinoids?

 

[Breakover]

have you figured out a way to extract the terps into a nice product like we are starting to see on the market while you are degassing or even before you extract the cannabinoids?

View Image

Sometimes my terp fraction smells good, sometimes it doesn't. I'd like to explore that further but I need a lot more space for additional equipment and whatnot.

 

[HG23]

Hey easystephen, how's it going with your Pope? Are you doing anything pre or post distillation to clean/scrub the oil?

Construction is almost done at the spot where I'm going to setup mine and I'm getting pretty excited.

It's great to hear about Breakover getting good quality in a single pass! That will really help kick up the overall efficiency of the process. I have always been told it takes a least two passes.

I have been reading about carbon filtering and saline washing as two pre-treatment techniques that may help achieve the "water" clarity that is popping up on the market. I believe carbon helps remove oil soluble (nonpolar) impurities and saline washing helps with the more polar pigments/impurities that are present, but I'm not sure. I have also heard GW and others mention column chromatography in relation to the same subject, but it seems like it may be hard to scale up. Column chromatography may also be useful in separating cannabinoids to allow for crystallization.

Does anyone have input or experience with any of these techniques?

 

[easystephen]

We have their 4" still, it really rips through material once you get it dialed in. There are a few things that we've found to be really critical in getting good results with the still. The most important is you need to get pretty much all of the volatiles out before doing a higher temp cannabinoid pass or the prevailing vapor pressure will be too high. Raoult's law is a mfer, study and understand it and your life will be much easier. We do a devolatilization pass before cranking up the temp and dropping the pressure for the cannabinoid cuts but you may be able to get away without it depending on your input material. What solvent are you using for extraction? What compounds distill is a function of whats in your feed material, some extraction techniques dissolve flavanoids and other diterpenes with similar boiling points to cannabinoids, this can give you a more amber distillate. We use warm ethanol extraction to produce the orange/amber distillate, cold ethanol gives a light gold/yellow. More selective solvents like butane or CO2 will give an even lighter color.

 

[HG23]

Interesting. I have been studying up on Raoult's Law the last couple of days and understand the importance of removing the low boilers. It just seems to make sense in general to remove as many impurities as possible from the starting mixture before distillation. For anyone interested in Raoult's Law it states the following: "The partial vapor pressure of each component of an ideal mixture of liquids is equal to the vapor pressure of the pure component multiplied by its mole fraction in the mixture." The way I'm interpreting it is the more low boilers (terps and ethanol) present in our starting oil mixture makes it's total vapor pressure higher which is counterproductive to a smooth distillation under vacuum.

I would really like to avoid having to do a devolatilization pass in the still. Both Breakover and Dean at Pope have suggested an extended session (an hour or two) in the rotovap at higher temps to help with this. What do you think about that?

I am going to start out with warm ethanol for the extraction solvent and add a chiller to the system when I can afford it. For dealing with large amounts of material, it seems like the easiest way.

Breakover, since you're running the condenser close to the temperature limit for distilled water (95C), are you using a mineral or silicone oil in the tempering unit? I'm looking at Polytherm M170. What about you easystephen, do you feel comfortable sharing your run parameters?

 

[Old Gold]

"The partial vapor pressure of each component of an ideal mixture of liquids is equal to the vapor pressure of the pure component multiplied by its mole fraction in the mixture." The way I'm interpreting it is the more low boilers (terps and ethanol) present in our starting oil mixture makes it's total vapor pressure higher which is counterproductive to a smooth distillation under vacuum.

Also, the less miscible/soluble/"like" compounds you have in general will make the whole process smoother and easier to control, because azeotropic reactions and boiling points under reduced pressure don't always act linearly in their numbers. In fact, they rarely do, due to things like heat of vaporization.

 

[Breakover]

Interesting. I have been studying up on Raoult's Law the last couple of days and understand the importance of removing the low boilers. It just seems to make sense in general to remove as many impurities as possible from the starting mixture before distillation. For anyone interested in Raoult's Law it states the following: "The partial vapor pressure of each component of an ideal mixture of liquids is equal to the vapor pressure of the pure component multiplied by its mole fraction in the mixture." The way I'm interpreting it is the more low boilers (terps and ethanol) present in our starting oil mixture makes it's total vapor pressure higher which is counterproductive to a smooth distillation under vacuum.

I would really like to avoid having to do a devolatilization pass in the still. Both Breakover and Dean at Pope have suggested an extended session (an hour or two) in the rotovap at higher temps to help with this. What do you think about that?

I am going to start out with warm ethanol for the extraction solvent and add a chiller to the system when I can afford it. For dealing with large amounts of material, it seems like the easiest way.

Breakover, since you're running the condenser close to the temperature limit for distilled water (95C), are you using a mineral or silicone oil in the tempering unit? I'm looking at Polytherm M170. What about you easystephen, do you feel comfortable sharing your run parameters?

No, just water, I do have to top it off periodically but it's not been an issue.

I tried doing a devol run a few times. It's effective but time consuming. I found the rotovap treatment to be faster and less labor intensive.

 

[Thomas@LRL]

No, just water, I do have to top it off periodically but it's not been an issue.

I tried doing a devol run a few times. It's effective but time consuming. I found the rotovap treatment to be faster and less labor intensive.

Do you just raise the heat bath temp and essentially decarb in the rotovap? In the past I have used a vacuum oven after the rotovap to achieve the same effect but I would prefer to do it all in one process prior to distillation if possible. When I took a distillation class the devol method was a hot plate and a heat gun with a lot of agitation but way hotter than I am used to decarbing. It seemed to do the trick though.

 

[easystephen]

Interesting. I have been studying up on Raoult's Law the last couple of days and understand the importance of removing the low boilers. It just seems to make sense in general to remove as many impurities as possible from the starting mixture before distillation. For anyone interested in Raoult's Law it states the following: "The partial vapor pressure of each component of an ideal mixture of liquids is equal to the vapor pressure of the pure component multiplied by its mole fraction in the mixture." The way I'm interpreting it is the more low boilers (terps and ethanol) present in our starting oil mixture makes it's total vapor pressure higher which is counterproductive to a smooth distillation under vacuum.

I would really like to avoid having to do a devolatilization pass in the still. Both Breakover and Dean at Pope have suggested an extended session (an hour or two) in the rotovap at higher temps to help with this. What do you think about that?

I am going to start out with warm ethanol for the extraction solvent and add a chiller to the system when I can afford it. For dealing with large amounts of material, it seems like the easiest way.

Breakover, since you're running the condenser close to the temperature limit for distilled water (95C), are you using a mineral or silicone oil in the tempering unit? I'm looking at Polytherm M170. What about you easystephen, do you feel comfortable sharing your run parameters?

The effect of Raoult's law is that you never get all of the ethanol and water out and in order to get it down to an acceptable level you have to use deep vacuum and high temps. The lower the mole fraction of ethanol, the lower the partial vapor pressure, this is why we run the rotovap at 85C and pull a really deep vacuum.

If you're doing warm ethanol extraction make sure you winterize very well before running anything through the still. If not, as soon as you remove the last of the water, all of the sugars and waxes will precipitate out and burn.

The difficulty with the still is maximizing yield (distillation rate) without burning anything, given the fact that we don't know the film temperature. I built a mathematical model of the still to help understand and predict performance. I'm currently implementing some automation in the temperature controller so that we can get maximum throughput. I'd like to add a feed pump to get better control as the feed rate effects everything, but the package is like $18k, in the mean time I think we can adjust for feed variations with automation in the temp controller.

 

[Breakover]

Do you just raise the heat bath temp and essentially decarb in the rotovap? In the past I have used a vacuum oven after the rotovap to achieve the same effect but I would prefer to do it all in one process prior to distillation if possible. When I took a distillation class the devol method was a hot plate and a heat gun with a lot of agitation but way hotter than I am used to decarbing. It seemed to do the trick though.

Yes, pretty much. High temp, deep vac.

 

[HG23]

Hey guys, I'm just checking in here to see how the Pope operators are doing. Anything new with you guys?

After a couple delays, I just received my ethanol extraction system and am beginning to produce crude oil. Soon it will finally be time to fire up the still. I have done a preliminary test of cold vs warm and it seems if the extraction is done at cold enough temps (-30C), there are no appreciable lipids dropping out of solution and I may be able to forgo the winterization step. Hopefully it works out and I can go right from the ethanol extraction system to the roto and then up to the still.

I'm also curious if anyone out there is using the feed pump system for their Pope. I have one on mine and am interested in any feedback you may have. I talked to Dean about it a couple months ago and I left the conversation not feeling very clear about how the system is supposed to be primed before use. I always thought gear pumps were self-priming. I will call him back, but in the mean time does anyone here know anything about that?

Also, I have the electric heat bands as the heating source for the evaporator core and seeing as the only temperature input to the controller is a single thermocouple under the lowest heat band, I'm expecting uneven heating right out of the gate. I was surprised they don't use a separate thermocouple and PID for each band (there are 6). Has anyone had issues with the heat bands?

Any other feedback would be appreciated.

 

[Breakover]

Hey guys, I'm just checking in here to see how the Pope operators are doing. Anything new with you guys?

After a couple delays, I just received my ethanol extraction system and am beginning to produce crude oil. Soon it will finally be time to fire up the still. I have done a preliminary test of cold vs warm and it seems if the extraction is done at cold enough temps (-30C), there are no appreciable lipids dropping out of solution and I may be able to forgo the winterization step. Hopefully it works out and I can go right from the ethanol extraction system to the roto and then up to the still.

I'm also curious if anyone out there is using the feed pump system for their Pope. I have one on mine and am interested in any feedback you may have. I talked to Dean about it a couple months ago and I left the conversation not feeling very clear about how the system is supposed to be primed before use. I always thought gear pumps were self-priming. I will call him back, but in the mean time does anyone here know anything about that?

Also, I have the electric heat bands as the heating source for the evaporator core and seeing as the only temperature input to the controller is a single thermocouple under the lowest heat band, I'm expecting uneven heating right out of the gate. I was surprised they don't use a separate thermocouple and PID for each band (there are 6). Has anyone had issues with the heat bands?

Any other feedback would be appreciated.

I'm just over here resurrecting old threads lol.

I'm sure the evaporator isn't heating evenly. A fluid jacket evaporator would be ideal, and I know pope does make one.

Beakerandwrench on IG has a pumped feed system available for the pope. It uses a peristaltic pump and controller to replace the manual needle valve. It's on my want list along with a fluid jacketed evaporator.

Still running my devol in the roto. I get the bath up around my targeted internal condenser temp on the pope(~95c) and pull as hard a vac as I can (~60mbar), running my condenser as cold as possible (~-20c). That way I have a better chance of getting anything out that would condense at my pope internal condenser temp and system pressures.