Large amount of solvent getting stuck in my closed loop system.

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Pimpernickel

Well-Known Member
I have a closed loop system with a 3'x18" material chamber with a cooling jacket around it. It reduces down to a 1 1/2" ball valve and I put some coffee filters in the reducer to stop any very small particles from getting through. I vacuum my loaded system down, place the collection chamber in an ice/salt bath, and put an isopropanol/dry ice bath in the cooling jacket then wrap with towels to try to insulate it. I'll fill with distilled butane until I get build a bit of pressure then I let it sit for 30-60 minutes. I open the valve and the solvent drops down into the collection chamber. After a minute or so I can let it sit there for 30 minutes and not get another drop of solvent, I can open the tank and run more solvent through and see about the same amount of solvent come out. I close the valve and finish the process but when I take the top of the column off for cleaning I'll always have 300-1000mL of solvent coming out of it. That's a very large amount and I cannot figure out why it's not draining into the collection chamber, any ideas? The cooling jacket gets down to -109F but that's well above the freezing point of butane, it can't be gelling at that temp can it?
 
dabbindylan

dabbindylan

Well-Known Member
Saturation of material..takes longer for perspiration to occur..perhaps its resdiual left in lines. Hope this was helpful
 
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Pimpernickel

Well-Known Member
Should I be leaving the valve open as I recover then as well?

For some reason I cannot post a link but if you google my extractor will show up.
HFS Sanitary Stainless Steel 304 3a , 0.5-5 LBS Closed Loop Reclamation Herbal Extractor , Passive / Active Closed Loop Systems (1LB (3x18" Dewax Spool) with Inline Display Windows
 
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cookie master

Well-Known Member
He described dewaxing setup. the material isnt at -109 the dewaxing column is. I think your main issue is that if the collection pot or recovery cylinder was as cold as that then itd suck better. The butane is chasing cold, but some gets stuck in the material column.
 
Fadedawg

Fadedawg

Well-Known Member
cookie master said:
He described dewaxing setup. the material isnt at -109 the dewaxing column is. I think your main issue is that if the collection pot or recovery cylinder was as cold as that then itd suck better. The butane is chasing cold, but some gets stuck in the material column.
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n-Butane turns to a gel long before -109C. That's one of the reasons we add n-Propane below about -30C.
 
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cookie master

Well-Known Member
I reviewed it and hes not doing a "true" dewax, hes cooling the material chamber. To dewax without alcohol I think you need a jacketed cylinder with a MUCH larger volume than the material. Run the material with multiple volumes of solvent, and collect it in the jacketed cylinder at subzero for a bit before filtering. Anyways- from what I hear its normal for the material to be a bit soaked and there be some waste. Thats why you dont run indoors.
 
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Fadedawg

Fadedawg

Well-Known Member
cookie master said:
I reviewed it and hes not doing a "true" dewax, hes cooling the material chamber. To dewax without alcohol I think you need a jacketed cylinder with a MUCH larger volume than the material. Run the material with multiple volumes of solvent, and collect it in the jacketed cylinder at subzero for a bit before filtering. Anyways- from what I hear its normal for the material to be a bit soaked and there be some waste. Thats why you dont run indoors.
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We run at -30C to -50C and when we open our system and remove the spent material, it is at less than 10% of LEL, but there are lots of other reasons to not run indoors unless it is in an extraction booth designed for the purpose.

After vacuuming to -29.5" Hg and backfilling with N2 twice, it is no more flammable when held to a flame, than the material was before extraction.

When you recover LPG under vacuum, you are simply removing the atmosphere suppressing its internal vapor pressure. Its internal vapor pressure is a function of temperature, which is low at subzero temperatures, so it doesn't boil as easily.
 
Aj struhar

Aj struhar

Active Member
Fadedawg said:
Details?
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I have a dewaxing column and a regular column in between the two I put a screen gasket and only keep the trim in the regular column dropping down the solvent only to the dewaxing column! From there I let it sit for a while then goes through a reducer with screen mesh on top and bottom and stainless steel wool and some unbleached coffee filters in between
 
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cookie master

Well-Known Member
Are your two columns the same size? Thats what I have but it seems like id need to run multiple volumes of the first cylinder nd the the 2nd isnt big enough.
 
Aj struhar

Aj struhar

Active Member
cookie master said:
Are your two columns the same size? Thats what I have but it seems like id need to run multiple volumes of the first cylinder nd the the 2nd isnt big enough.
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Yes both columns are exactly the same size! Not sure what you mean by run multiple volumes? Unfortunately I have a top feed so I dumped for a little bit turn it off let it sit and then dumped again till I have nearly almost emptied my solvent chamber! @Fadedawg would love any advice you can give on how I'm currently running my system

Bvv 5lb with dewaxing column on bottom with mesh screen gasket in between the regular column. I also use a unbleached coffee filter on top of that mesh screen in between. Then below dewaxing column is a reducer down to 2 in to a ball valve. At the bottom of the reducer is a 2 inch screen gasket also and in the reducer I use stainless steel mesh with coffee filter on bottom and top.
 
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