Re-dissolving Extracts for Remediation or Re-crystallization

All,

Got another question for everyone. How do you guys re-dissolve your extracts if they test hot for pesticides and need to be CRCd or if you need to re-crystallize?

And please don’t tell me you throw it back into your static evaporation column on your extraction machine and heat it as much as you can before your blow off valves are overloaded, tried that and it’s both highly ineffective and a massive pain in the ass because you just clog up your system and really achieve almost nothing.

Thanks!
-Butane

2 Likes

I use the hot vapor from my recovery pump to agitate the oil to get it to efficiently dissolve. It can be done in a material column or collection . Biggest thing is not trying to dissolve too much at once start with 500-1000 grams to get the hang of it . Clogs are inevitable when redissolving having a plan on how to fix the clog is essential like spare hoses and bypass . Also you need to start with room temp butane idealy preferably straight n butane because it works best . Isobutane will work but require higher temps and longer

5 Likes

Reflux with butane in a jacketed collection vessel.

5 Likes

I had a 6x48 clog with 4000g of dark stuff i was re running and tried everything you could possibly imagine to un clog it . Even let it sit over night full waiting for it to dissolve . Had to flip the tube upside down on the rack to get the rest of the butane to the collection from the top liquid fill. Then scrap out an 8" thick wad of oil clogging the entire tube . I hate but also love re runs .

1 Like

If you redissolve clean thca and recrystallize let me know if you get Medusa stones or not

5 Likes

Several ways to do this …

I used to put my dope into a filter sock and hang it from my shower head in my material column & just run the loop until the sock was empty…until I got a 50L stainless jacketed reactor and started doing it the way @murphymurri does it, which is putting it into your collection tank, soak, recover & repeat while keeping it wet. It helps to have a valve at the bottom of your collection, without that the hanging sock method was the easier for me

It really depends on how much your trying to redissolve

4 Likes

I can dissolve 2000gs at a time in 6x48 in about 1-2 hours if things go smooth with no clogs . The hot vapor agitates the material and heats it downside you need a recovery pump . After trying tons of ways to dissolve i really prefer this tek . Our system was built to do this with ease . All you need is a T and ball valve with a line after the pump. One of the advantages of having an passive/ active hybrid system. If you want to go crazy you could just load up you collection and use the spray valve at the bottom to pump the hot vapor to dissolve everything . It just nice on a 6x48 cause you can put a sight glass on to visually see what is going on

1 Like

Throw the extract in a sock to prevent clogging and use a fritted filter plate underneath the column to catch the sock

5 Likes

Why does isobutane tank longer to disolve something versus butane?

Bottom injection only using hot solvent. Havent clogged since

1 Like

N butane is a slightly more aggresive solvent and is better at dissolving compared to isobutane which is more similar to propane.

1 Like

I initially bottom fill solvent so the first thing that hits the sintered disc is clean solvent . But i also flush with clean solvent from the top as well . The reason i get clogs is cause i run crx from media bros so the crc has to be -10 or colder to work . So i run a coil after the material column to chill the solvent before the crc. This always clogs cause the intial solution is so thick it can clog when sub zero . If you have a jacketed crc or use regular media you should be fine

Always good to prewet the crc with solvent too

I didn’t see this mentioned, but powderizing the THCA makes this process go quite a bit faster.

7 Likes

Yep, bubbling hot vapor in through the bottom while pulling off the top is very effective.

See: Re-dissolve BHO for CRC

3 Likes

I have a couple of theories I’d like all of your opinions on. It’s a bit of a read.

I have been deliberating on different methods for re-dissolving extracts for remediation or re-crystallization and have thought up a couple of alternate options that could potentially work, while also preventing the need to use extraction machine time to do so. It’s a bit of a read so buckle up.

The Problem

The largest issue with using extractor evaporation columns to dissolve extract is that once you’ve added the extract and solvent to the column, there is no way to agitate or break apart the extract in order to expose more surface area to the solvent to speed up the dissolution process (Sounds like you guys bubble vapor through the solution to agitate slightly). Having a sphere or pancake of extract in the bottom of the column means you have what is essentially the smallest surface area to volume ratio possible in physics (a sphere) of extract exposed to solvent. If we can break that up into multiple spheres/chunks, you begin to exponentially increase the surface area of extract exposed to the solvent, therefore exponentially decreasing the time it will take to dissolve.

Beyond increasing surface area, the only other way to speed up the dissolution of the extract in the solvent in a static container is to heat up the solvent therefore increasing its solubility, and because we are using Propane/Butane which already have very low evaporation points, that means we would need to reach some pretty high pressures in our columns in order to warm the solvent up enough to positively impact the solubility of the extract. Because we are limited to our blow off valves on the evaporation columns, we would likely not be able to get the solvent above 70 degrees Fahrenheit before we reached the blow off limitations of our columns. This means heating is also not a practical solution to reducing dissolution times within an extractor.

Option 1 - Physical Agitation

This method is purely speculative and I have not tried it but also would be essentially a negligible cost to attempt.

We have a small 5 gallon stainless steel solvent tank with a removable lid and a rounded bottom that is currently not in use. We could purchase an explosion proof Drum Rotator with an adaptor for 5 gallon buckets that would work nicely to safely and continually agitate the tank and vastly increase dissolution speed. Additionally, we could purchase 2-3 stainless steel 3" diameter ball bearings and place them inside the tank with the extract to further increase dissolution speed and agitation.

Once dissolved, we could pass the solvent and extract solution through a CRC column to remediate, and then recover the solvent in our extraction system under normal operating conditions. We could also do the same if the goal is re-crystallization instead of remediation.

Pros:

  • Cheap to perform a proof of concept
  • Reduce loss of extraction machine time

Cons:

  • Relatively expensive to implement on a commercially viable scale
  • Need a space for the drum rotator, not sure if it would need to be inside the C1D1
  • Would still need to utilize some extraction machine time for the solvent recovery

Option 2 - Alternative Solvent (Pentane)

Pentane is a hydrocarbon like Propane and Butane, however it has a much higher evaporation temperature, and will remain a liquid at room temperature due to that fact. This makes it much easier to heat up in order to increase temperature and therefore solubility, because the pressures required to reach higher temperatures are much lower than would occur with Butane or Propane. This means we could potentially fill a small 5 gallon tank with extract and pentane, then using a 5 Gallon Bucket heating blanket, we could warm the tank to the point where the extract would dissolve much more readily into the pentane (around 100F), and potentially even without any agitation. Then we could pass the pentane and extract solution through a CRC column using nitrogen for head pressure into a second tank. We could then utilize a rotary evaporator to recover most of the solvent, leaving only enough solvent in the solution to perform the super-saturation crystallization process in our vacuum ovens if that is the desired outcome.

Pros

  • Also cheap to do a trial run, just need a tank heating jacket and some pentane
  • Eliminate any need for extraction machine time

Cons

  • Would need to use rotary evaporator to recover solvents
  • Would likely result in a higher loss of terpene content versus above method due to higher evaporation temperatures necessary for the solvent recovery process (Not a concern for THCa isolate)

Option 3 - Combine the above two methods

Assuming both methods show positive results, one could ultimately combine the pentane dissolution and heating with a physical agitation to decrease the dissolution time significantly. By heating a pentane and extract filled tank with a tank jacket then removing the jacket and placing the hot tank on a roller, you could potentially see very low dissolution times compared with using either of the above two methods on their own. This would also isolate the process from the extraction machine, maximizing our ability to produce in the meantime.

Also, both methods may be better for one thing or another. For example if keeping terpene content intact is a large concern, it may be best to use Propane/Butane for the process. If large diamonds is the goal and terpenes are not a factor, utilizing pentane may be the best solution. It’s possible that these variables could be only applied to specific products based on the desired end result.

What are your thoughts on these two methods compared to some of the methods you’ve provided? Do you think they have any advantages or disadvantages or just flat out wouldn’t work at all? Looking forward to your replies.

Is this a guess or is this for real :thinking: gotta get it hot mane. I don’t ever see over 50 psi

True for propane but not butane. Here is a handy little chart You can see with just butane you’ll be under 50psi at 110f and at 70f only at 17psi.

2 Likes

It’s an estimation based on the evaporation temperature vs pressure of propane. The more you heat it in a closed cylinder, the higher head pressure you’ll build. You might have a vapor temp higher than 70F but if you’re using propane the solvent itself won’t be much over 70F unless you’re over 150psi. And evaporative cooling will further suppress your ability to get those temps much higher than that while staying under 150psi

2 Likes

I dissolve it in a higher alkane like a normal human being

1 Like