Active closed loop extractor late with drops and Interesting end product ( pure propane )

[WrigleysHaze]

Hi,

I have a 2 lbs closed loop extractor active (but it only fits max 1.5 lbs) and I have a few basic questions and problems. Unfortunately, I am currently working without pressure support, but this should change in 1 - 2 weeks.

My biggest problem is that after rinsing, when there is already more than approx. 70% in the collecting tank, the rest of the solution is still in the material chamber and keeps running out in small waves. I could understand constant running or dripping, but there are always a few ml and then a short pause and then something comes out again, etc.

That's why I usually flush 2-3 times and add about 13.5-18 lbs per flush. 100% propane @ -22°F to -40°F.
I get ~50g on the first wash, ~15-20g on the second and 5-10g on the third.

Is this due to the lack of pressure support or am I using too little solution or is it normal that you can/should wash several times?

and finally, could someone tell me something about my product?


In Collecting chamber


After scratching together


After 48h in vacuum at ~100°F
What did I do there and why is it so different, should I mix it?

 

[Fadedawg]

May we see a picture of your system?

I typically run three column volumes through in one shot. Is your collection tank big enough to hold three column volumes?

 

[WrigleysHaze]

Looks like this, without cooling coil.

Yes, I also run this amount through and after that, you don't do a second run with the same material?

 

[Dirt_McGirrt]

Second runs should be pointless unless there was channeling. All you'll get is junk mostly. Are you soaking the material at all or just dumping it when it fills? Do you sub zero freeze everything? Is it dry or fresh? Is there a filter in that setup?

Is there a sugar daddy out there giving away closed loop systems? I was barely able to afford a small closed system, not closed loop. I consistently get sugar/crumble/badder premo stuff. People out here like "first time how do I do drive a car" with a Cadillac.

 

[WrigleysHaze]

What do you mean by channelling?
I just run it through and it's dry material and everything is at least - 30°C (- 22°F).
The material is in a 35 micro filter sock.

 

[Fadedawg]

View attachment 5276111
Looks like this, without cooling coil.

Yes, I also run this amount through and after that, you don't do a second run with the same material?

What are your column and collection tank dimensions? Hard to tell from a picture, but it looks like a 2" X 24" column, which would hold less than a pound of material. I infer your system is larger.

You said your system was active, but the one in the picture has no pump. Does your system have a pump?

How are you preparing and packing the material in the sock?

What is your extraction process? Are the material, the column, and Propane at <-30C?

In answer to your question, channeling is where uneven material packing allows the LPG to find easy routes (channels) through the material, thus not adequately extracting the material outside the channels.

In answer to your second question, after flooding the columns with three volumes, there was not enough remaining essential oil to justify repacking and re-running.

Looking at your product pictures, I suggest blending it. It also looks like a low yield for 1.5lbs of material. What was the material?

We prefer a 70:30 or 50:50 LPG blend, vis a vis straight propane. Are you using 100% propane for a reason?

 

[Turpman]

Sounds like the propane gravity drains? Is gas slowed to enter the top to replace the liquid propane as it's draining? Sounds like it's causing vacuum above when draining.

 

[WrigleysHaze]

It is a 4 x 24 column and an 8 x 24 collection bin.

Yes, I have a Bosch RG 4.0 certified for propane and so on.

I grind it with a kitchen chopper coarse, ready for a joint, so not too fine.
Then I put it in a nylon sock/strip.
I have one that fits perfectly and one that is a bit loose.

So the perfect packing is that I put the sock into the material chamber and fill it with the same pressure as I fill it, so that I don't have any air holes and everything is as uniform as possible.

The extraction process looks like this:
I store the material chamber (with material) and propane for at least 24 hours at -30°C to -40°C so that everything is deep-frozen.
Then I take the material chamber out and put it on the collection container (this is vacuumed for at least 30 minutes), when the material chamber is on top I also vacuum it and connect the rest of the hose and the propane and leave the whole thing to vacuum for another 10 minutes until you hear the pump running quietly.
Then turn off the vacuum pump and slowly open the ball valves and listen to the gas flow
Then I switch on the recovery pump and watch the propane flow through. Always magical, in my opinion.

The propane tank is then placed in ice water during recovery and the collection tank is placed in warm water (max +40°C) so that the whole thing can move forward.

Bad old trim and the under third of the ladies. and i got 82g yield from 600g material is 13.67% sounds really good to me or what do you get out of it?

First of all propane is much cheaper for me and easier to get, secondly I have bad material and what I have read is that propane absorbs less pollution and above all less chlorophyll.

The question I ask myself with a mixture is whether my freezing point rises or falls. pure propane has -42°C. What do your blends have?


Yes, the garvitation still flows off, sounds logical what you say, like holding a bottle upside down only it is still full of flowerpower

I'll get argon tomorrow and can then try the whole thing with pressure.

I will then decant the old material into the larger sock and then wash it 3 times to see what is still in there and what a real run will be like.

Edit: Iso butane or normal butane, which do you prefer?

 

[Fadedawg]

It is a 4 x 24 column and an 8 x 24 collection bin.

Yes, I have a Bosch RG 4.0 certified for propane and so on.

I grind it with a kitchen chopper coarse, ready for a joint, so not too fine.
Then I put it in a nylon sock/strip.
I have one that fits perfectly and one that is a bit loose.

So the perfect packing is that I put the sock into the material chamber and fill it with the same pressure as I fill it, so that I don't have any air holes and everything is as uniform as possible.

The extraction process looks like this:
I store the material chamber (with material) and propane for at least 24 hours at -30°C to -40°C so that everything is deep-frozen.
Then I take the material chamber out and put it on the collection container (this is vacuumed for at least 30 minutes), when the material chamber is on top I also vacuum it and connect the rest of the hose and the propane and leave the whole thing to vacuum for another 10 minutes until you hear the pump running quietly.
Then turn off the vacuum pump and slowly open the ball valves and listen to the gas flow
Then I switch on the recovery pump and watch the propane flow through. Always magical, in my opinion.

The propane tank is then placed in ice water during recovery and the collection tank is placed in warm water (max +40°C) so that the whole thing can move forward.

Bad old trim and the under third of the ladies. and i got 82g yield from 600g material is 13.67% sounds really good to me or what do you get out of it?

First of all propane is much cheaper for me and easier to get, secondly I have bad material and what I have read is that propane absorbs less pollution and above all less chlorophyll.

The question I ask myself with a mixture is whether my freezing point rises or falls. pure propane has -42°C. What do your blends have?


Yes, the garvitation still flows off, sounds logical what you say, like holding a bottle upside down only it is still full of flowerpower

I'll get argon tomorrow and can then try the whole thing with pressure.

I will then decant the old material into the larger sock and then wash it 3 times to see what is still in there and what a real run will be like.

Edit: Iso butane or normal butane, which do you prefer?

Is the inner column 4” or is that the size of the jacket. With ground material, I typically get around 4.1 grams per cubic inch of column volume, so a 4” X 24” should hold closer to 2.5 lbs.

Your system is also a top flood, so unless it also has a shower head on top, with a 4” column you are not getting full wetting of the surrounding material at the top of the column. I flooded from the bottom and overflowed from the top to avoid that issue.

Packing a column or a sock uniformly is more critical with a top injection than a bottom flood and I never used a sock. We cleared the columns with a blast of compressed air.

Those times I’ve been involved with a system using a sock, we compressed the material into a tube with a pneumatic ram, and then opened a knife gate valve at the end of the tube and shoved that into the sock. How ever you do it, uniformity is critical with a top injection.

I suggest adding a compound vacuum gauge and exhausting your system to -29.5” Hg, rather than until the pump runs quiet.

Other than listening to gas flow, how do you tell that you have injected three volumes of LPG?

Yield is highly dependent on material and 13.67% from bad old trim is certainly in the ballpark. We typically got 18 to 25% from prime bud with trim, and about half that for trim.

Price is certainly a factor, but Chlorophyl is polar, due to the magnesium ion in its tail, so not typically an issue with the non-polar alkane solvents at -30/40C.

A 70% n-Butane:30% n-Propane mix reaches zero vapor pressure at about -10C.

You might consider Nitrogen, which is way cheaper than Argon and is also inert.

I heated my columns to 150F following injection to drive off the remaining LPG, and with a recovery pump, I never needed any pressure assist to clear them.

I’ve used hot vapor assist when injecting n-Butane at -50C. I simply connected the vapor ports of the 0C/32F injection tank to a second tank at 110F. Introducing a non-condensable gas into a pumped system can be problematic, unless you bleed it all off before recovery.

Same with not removing it all before injecting the LPG, because If it gets into your recovery tank, it drives the pressure up and recovery slows to a crawl.

I used Instrument grade n-Butane and n-Propane, which worked well. I redistilled and filtered them once for mystery oil and got about 99.98% purity with regard to molecules larger than C-4.

I’ve used Iso-butane, but saw no advantages, and is more expensive here. How does the price and availability compare in your neck of the woods?

 

[Dirt_McGirrt]

you should try vacuuming the column before freezing and maybe not freeze a full 24hrs. try 12hrs. water freezes around trich heads after too long especially if there's atmosphere in the column.

i'm not a mad scientist like Fadedawg, here, but def try a blend instead of straight propane. Even going to straight tane I prefer the blend.

 

[WrigleysHaze]

The inner column is 4 large, so 5 litres in volume.

The shower head will be delivered in 2-3 months...
I always stuff the nylon sock all the way to the top so that, in my opinion, the LPG should be distributed quite well.

Flooding from below is a great idea, but it's not quite clear to me how you get the column empty.

So the colder the better.

I have two pressure gauges but I only manage -29" Hg, only on good days do I manage -29.5" Hg when the pump runs for a long time. and apart from running for longer or buying a bigger pump, there's not much I can do, is there? ( my pump has 5 cfm & is two stage )
I have tow windows in the LPG tank, so I can see it and I also have a scale.


So the colder the better.
But why do you all use so much butane? I heard it's better for shatter, but I didn't like the high boiling point and the low pressure. But I have to say that my product was completely different and "better". I used the old material (3 runs) to make 5.5g of the finest dark Carmel shatter. No budder mix like on the pictures above & that only thanks to 800g n-butane which I added to the ~ 8000g propane.

Yes, I will buy nitrogen soon, but right now I only have argon at hand.

When you heat the column to 150F you mean the material column right?

Or do you mean with the hot steam that you build up pressure from the LPG in a second tank and then feed it into the LPG tank so you don't have any problems with venting / rising pressure / slow recovery. If so really brilliant if you have a second tank.

I can only get normal LPG and then have to filter it. I have sent it through the system 3 times empty and each time a molecular sieve with 4 angstroms, so everything should actually be out for me.

The price difference between iso & n butane is so small that I will treat myself to the iso because it has a little more pressure and the boiling point is already at -11.5°C. I will fill the column beforehand.

Have you tried other alkane mixtures, like ethane or petane, just as small admixtures?

I will fill the column beforehand and then draw a vacuum and freeze it for 12-24 hours. the water under atomic spheres is a really good point.

Thank you guys it is a real pleasure to talk shop with you.

 

[Fadedawg]

The inner column is 4 large, so 5 litres in volume.

The shower head will be delivered in 2-3 months...
I always stuff the nylon sock all the way to the top so that, in my opinion, the LPG should be distributed quite well.

Flooding from below is a great idea, but it's not quite clear to me how you get the column empty.

So the colder the better.

I have two pressure gauges but I only manage -29" Hg, only on good days do I manage -29.5" Hg when the pump runs for a long time. and apart from running for longer or buying a bigger pump, there's not much I can do, is there? ( my pump has 5 cfm & is two stage )
I have tow windows in the LPG tank, so I can see it and I also have a scale.


So the colder the better.
But why do you all use so much butane? I heard it's better for shatter, but I didn't like the high boiling point and the low pressure. But I have to say that my product was completely different and "better". I used the old material (3 runs) to make 5.5g of the finest dark Carmel shatter. No budder mix like on the pictures above & that only thanks to 800g n-butane which I added to the ~ 8000g propane.

Yes, I will buy nitrogen soon, but right now I only have argon at hand.

When you heat the column to 150F you mean the material column right?

Or do you mean with the hot steam that you build up pressure from the LPG in a second tank and then feed it into the LPG tank so you don't have any problems with venting / rising pressure / slow recovery. If so really brilliant if you have a second tank.

I can only get normal LPG and then have to filter it. I have sent it through the system 3 times empty and each time a molecular sieve with 4 angstroms, so everything should actually be out for me.

The price difference between iso & n butane is so small that I will treat myself to the iso because it has a little more pressure and the boiling point is already at -11.5°C. I will fill the column beforehand.

Have you tried other alkane mixtures, like ethane or petane, just as small admixtures?

I will fill the column beforehand and then draw a vacuum and freeze it for 12-24 hours. the water under atomic spheres is a really good point.

Thank you guys it is a real pleasure to talk shop with you.

At 1.5 lbs of ground material in a 302 cubic inch column, your packing density is only around 2.25 grams per cubic inch, which is light and promotes channeling. At 2 lbs, your density would be 3 grams per cubic inch, which is still lighter than we packed our columns.

We packed ground material at around 4.1 grams per cubic inch volume and 3/8-1/2” broken up buds at around 3.8 grams per cubic inch.

With a bottom flood or a bi-directional flood, there is a valve at the bottom of the column that allows you to dump the column contents and vacuum it out, after flowing three column volumes.

In the bi-directional flood, we flowed two volumes from the bottom and rinsed one volume from the top.

Attached is the original Terpenator schematic, showing the bottom flood feature and valving. I’m having difficulty opening my CAD files at the moment, so you will have to wait on the bidirectional schematic.

Cold is good, but there is a point of diminishing returns. The object of cold is to slow down dissolution of all of the molecules.

It slows down the longer chain molecules more than the shorter ones, so it gives you a longer window to dissolve the targeted C-10 through C-22 terpene and cannabinoids, without significant pickup of the ~C-29 plant waxes, C-40 Carotene, and the C-55 Chlorophyll molecules.

It avoids non-targeted elements, rather than requiring their later removal, which allows you to produce a more aromatic non-winterized terpene rich end product.

An alternative is in-line dewaxing, which removes the plant waxes, but doesn’t remove the Carotene or Chlorophyll.

Nothing wrong with using Argon other than price, and some advantages, in that it is heavier than air, so floats any contaminating atmosphere.

My material columns were jacketed and after I finished flooding and opened the lower dump valve, I pumped 150F water through the jackets. That drove off the residual LPG, which was recovered by the pump,

I backfilled my system with Nitrogen after LPG recovery, and after baking at 150F and being under 29.5” Hg, plus the Nitrogen backfill, the material was below LEL for LPG.

Hot vapor assist is different than the column heat. It puts head pressure on the LPG mix used for injection, while the LPG is cold enough to not have enough head pressure in the tank to push it through the system. The advantage over using Nitrogen assist, is that you don’t have to later purge them out.

I’ve extracted with Pentane, Hexane, and Heptane, but not mixed with my LPG. I’ve instead made every effort to remove all molecules larger than C-4 before extraction as Mystery Oil.

 

[WrigleysHaze]

Okay, I have now also packed more strongly with ~3 g per cubic inch. But I still didn't get more yield, again ~ 55g, which I think is low because I took 1/3 more material.

The bidirectional flooding is a great idea. I will also expand my system with it or buy a bigger one with bidirectional so that I have more solution. Because my tank can only hold 2.8 times the volume.

Do you let the material soak in the column when it is full of solution? Or how long does it take to fill a column with LPG?
I'm thinking of letting the material draw for a short time, as far as I can, with the flooding from the top. I have also heard that the material piston is supported with vibration during soaking to increase the yield.

Thanks for the drawing, it helped me a lot.

At what point does the cold no longer help me? From what I have seen on youtube so far, professionals work with cooling devices, most of which are set at -50 to -60°C, to cool the coats. So I thought the colder the better.

So the solubility of the C molecules depends on the temperature as well as the soaking time and the mixture of the LPG right?
So it's probably hard to say how long it will take to get the desired product or maximum yield.

I have nitrogen for now and I'll have to see if I can buy it cheaply with the superheated steam. Because pressure support simply has to be there.

Ah okay, so that's Mystery Oil.
And I am quite sure that this is the case, but is it possible that the propane is recovered first from the solution in the collection tank and then the n-butane? Because in the end, the recovery process takes a long time if you don't add heat.

 

[Fadedawg]

How long it takes to flood the column, depends on the size of the column. The WolfWurx Mk IVC or VC both take about 45 seconds to flood a 4” X 36” column. The way we measured three volumes, was to time when the LPG overflowed the top of the column, and continue to flood twice that long for the remaining two volumes.

Both of those units had inline sight glasses to tell both when it overflowed and the color of the LPG exiting the column.

We didn’t soak, we either ran three volumes from the bottom, or two from the bottom and one from the top, but we could tell how we were doing by the color of the LPG exiting the column.

I ran the Terpenators at -30 to -50C with good success. I used counter flow heat exchangers with LN2 to lower the injection temperature to those ranges, and kept my recovery/supply tank at 0C/32F.

Yes, the solubility of the molecules involved are a function of temperature, time, and flow. Just soaking places the solvent and solute in contact, but as the solute dissolves, the solvent becomes less pure/concentrated and the solute at the solvent/solute interface does as well, so the process slows down. You need enough flow to keep that boundary layer refreshed.

The easiest way to determine when you have passed enough LPG through your column, is to watch the color. With a bottom flood system, you can simply put a sight glass in the column overflow.

When recovering an LPG mixture, either passively or with a pump, the Propane boils off first through fractional distillation.

We heated the collection pot to 85F, not to drive off the LPG, but to replace the refrigerative effect of boiling off the LPG under vacuum. Without heat, the solution temperature drops to the boiling point and slows down the recovery process.

 

[WrigleysHaze]

I also was able to wash once from the bottom and once from the top today.
Have the first rinse from below the whole still pull 4 min, then ls I rinsed from above was the LPG white. However, this was also the case with the other runs and when I then washed the next day, I have trozdem again get extract out.

What amazes me is that I always get 50-60 g out of the first run and the second 25-50g, but the LPG is still white at the end of the run.
The penultimate run with loose buds 1.1kg has resulted in 4 runs 55/50/27/10 g, I find quite good but I had to wash the whole 4 times and I got the first time butter, #2 was shatter, #3 was crumble, #4 was shatter again. which I find kind of funny because the process was exactly the same, but also stupid because would be nice to always produce the same or at least targeted.

And then why did everyone like to use mixes so much? I don't understand. Propane has more pressure and boils earlier.

Could it be because I keep the material column frozen and do not heat it (during the recovery process) that this leaves behind quite large amounts of extract and I have to wash it several times?

And very nice system you have there

 

[Fadedawg]

What method did you use to flood from both directions?

At subcritical pressures, Butane does a better job extracting the targeted elements than Propane, but has no pressure below 0C. Propane adds that pressure. Propane is also typically used in SCFE systems.

Some systems use butane at subzero temperatures and force it through with nitrogen or hot vapor.

Chilling the column during recovery would definitely be counterproductive. You might consider draining it and running hot water through it during recovery. I ran WolfWurx columns at 66C/150F during recovery using hot water but used closed jackets designed for that purpose.

Thank you, that was the only Mk IVB that we built, before changing to the Mk IVC configuration, with different counterflow exchangers and pressure pot.

Here is a picture of a Mk IVC recovery pot and the one Mk IVB that we built.


First run from Mk IVC SN 00013.



Mk IVB ready for delivery

 

[Fadedawg]

PS: The product picture reflects the "Cotton Candy" recovery process, by which the LPG is recovered to the "blurpy" stage and then the high vacuum pump is turned on, which expands the oil into foam. Bubble walls are the thinnest possible wall thickness from which to purge, so the material retains less residual solvent.