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question regarding filtering/decanting bho winterized in ethanol

Discussion in 'Concentrates & Processing' started by endora, Feb 15, 2014.

  1. endora

    endora

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    I've been through most of the threads here and have a question about filtering after winterizing. The waxes/lipids are not being removed with a coffee filter as outlined below. They just re-dissolve.

    I have also tried using a separation funnel, and the waxes/lipids quickly plugged it and I was forced to siphon off the liquid instead. I now question if a syringe filter works that well either. I haven't tried one yet because they seem really expensive.

    Graywolf was saying:
    "As far as filtering, I prefer a 0.45 micron or a 0.2 micron syringe filter, but got good results with a coffee filter until Joe turned us on to syringe filters. We have picked both the syringes and filters up off of E-bay, as well as from our local scientific supply store.

    I heat 190 proof ethanol to boiling and pour it in the oil, stirring vigorously until it is fully dissolved. I pour that through a coffee filter into a container like a fruit jar or bottle, and place in the freezer for a minimum of two days.

    You will notice a light colored material starting to coagulate and precipitate out. If you leave it long enough, it will sink to the bottom of the container.

    I then pour that mixture through a coffee filter, and the light beige waxes are left behind on the filter."

    What I have discovered is this: after two days of winterizing at 0 degrees F as specified I decant most of the liquid and run it through a coffee filter. For the remaining bit of liquid and all of the sediment I use a fresh coffee filter. And the waxes/lipids etcetera simply re-dissolve and pass right through the coffee filter into the batch. They aren't left behind on the coffee filter at all. Note that I've run at least 8 varieties through this process now; none of them filter.

    I verified that this is what actually happens by then re-freezing the 'filtered' solution again; the solids are all still there.

    This is driving me insane at this point. I need an effective way of getting ONLY the solution and leaving behind the waxes/lipids. I had hoped the sep funnel was the answer, but it plugs up every time.

    Any advice appreciated. How fine would a filter have to be if this stuff is still easily passing through a 1/2 micron coffee filter?
     
    Chronic Monster and ftwendy like this.
  2. Hmmmm I always get residue of waxes and various size globs left behind in my coffee filter, but I discard them.
    You could try vac assist on your sep funnel.
     
    Wavegem likes this.
  3. I'm certainly no expert on this matter, but maybe some photos would help. Perhaps what you're seeing aren't actually waxes.

    -- iCultivate --
     
  4. Dunge

    Dunge

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    Any chance you could chill the filter?
     
  5. endora

    endora

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    Hi guys.

    I saw a milky-ish flow in the filtered liquid so I suspected that the waxes/lipids were going back into the liquid through the filter. Possibly due to it warming, but I do it right out of the freezer, so... When I re-winterized the already-winterized and then filtered ethanol, there those same solids are at the bottom again. Some of them do end up staying on the filter; but not nearly all of them.

    A vac-assist is just gonna pull them through more effectively, but maybe with a lab-grade filter. I'll look into that. Icultivate: I can't post pictures of something that isn't there. When I re-winterize? There it is. It looks just like after the first winterizing. Nothing confusing about it.

    I am converting this into oil for cartridges so this step is critical. My first couple batches where I didn't worry about the filter problem ended up eventually congealing and the cartridges failed. My later batches where I siphoned off from the top and filtered that have all worked great and re-winterizing shows no remaining waxes etc.

    I've decided a few things since my first post. Syringe filters seem like a worthy investment; I'll go for the .22 micron ones. I guess I could also try a different brand of coffee filters. I am also going to check the actual temp of my freezer; maybe it's not fully down to zero. I doubt that 10 degrees is much worse than 0 degrees but maybe so?
     
  6. If the product is resulting in the cartridges failing from it congealing, then I guess it does sound like the waxes are still present. Sorry I can't be of help, but there are plenty of more knowledgeable farmers here who can help you more than I. I've only dabbled with making oil and never tried to refine it to this level as yet.

    I think Graywolf or Wavegem would be the best people to ask.

    -- iCultivate --
     
  7. endora

    endora

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    Hey, thanks anyway. Any input helps. I'm just doing small batches of cartridges for my patients. Pen vapes are a game changer for them.

    Part of me wonders if anyone else has ever re-winterized to see just how effective their filtration process actually works...? but honestly I bet a syringe filter will solve the problem for me. I would love to have a .25 micron stainless filter mesh, though: get that frozen and you'd be good to go for sure.
     
    germinator likes this.
  8. Wavegem

    Wavegem

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    Save yourself a headache and do what germinator said. Get a vac assist filter at .25 micron. You will be happy you did. Those syringe filters suck! Even .45 works which is what I use. If you still have wax in your product you need to freeze it for longer at least 48 hours.
     
    Chronic Monster likes this.
  9. If I understand you correctly, you are talking about filtering the dregs, not the main solution.

    I've never tried to do them separately, I either squeeze the remaining liquid through the first coffee filter or let the vacuum pull it through a #1 Whatman. We then save those filters, and extract them in batches with ethanol, to salvage residual oil.

    My first question would be what temperature were the dregs and what temperature was the filter, when they went back into solution and ran through your filter?
     
  10. Syringe filters are not a good choice for dewaxing, because they clog so fast and don't have a lot of surface area. Better to use vacuum filtration first, to remove the bulk of the material.

    We vacuum through a #1 Whatman lab filter first, and sometimes filter at 0.45 micron, before 0.2 microns. The 0.2 micron is for critters and spores, not wax.

    It is also for small batches, because the effort can be significant.
     
  11. Water produces a milky flow.
     
  12. You need to do the filtering inside the freezer. Freeze the filter and glass it's going into to. Everything is warming up during the process and the solids are turning back into liquids.
     
  13. endora

    endora

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    Hey, thank you for the responses. So it turns out I just had crappy coffee filters. Duh! I got some premium cone ones and the filter was covered with goo after. Huge win. So: yay!

    That said, I'm going to order a vacuum funnel set-up and some #1 Whatman lab filters. I'm small-craft-batch all the way so why not.

    Thanks again.
     
    Graywolf likes this.
  14. just want to add to this conversation incase people like me are still googleing and reading stuff.

    regular coffee filter is 25 microns
    #1 Whatman filter is 11 microns

    I myself will filter 3 times

    first time with 1 coffee filter @ 24 hours in freezer set at -6F
    second time with a 10 micron filter @ 36 hours in freezer set at -6F
    third time with a 2.5 micron filter @ 48 hours in freezer set at -6F