What's new
  • Happy Birthday ICMag! Been 20 years since Gypsy Nirvana created the forum! We are celebrating with a 4/20 Giveaway and by launching a new Patreon tier called "420club". You can read more here.
  • Important notice: ICMag's T.O.U. has been updated. Please review it here. For your convenience, it is also available in the main forum menu, under 'Quick Links"!

lipid not settling to the bottom during winterization?

B

ButterCup

Member
I have tried winterizing at 0F, -20F, even -115F. But the lipid are floating around in the solution, which is making filtering extremly slow even with vacuum assist.

Anyone know what is going on.

BTW I am heating up the ethanol and dissolving all the bho evenly before i put it in the freezer.

Thanks in advance for your help.
 
Gray Wolf

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Typically at 48 hours, they would be out of solution, but still suspended.

Try using a sock filter, with more surface area, or using a paint brush to keep brushing the accumulated was off the surface of the membrane filter, to keep the pores open.
 
T

thegreenman91

Member
Hey Grey Wolf... Is there a good centrifuge for our industry? The largest I can find is 6x 1000ml. Is there a centrifuge with a large sized single bucket design that could effectively be used for winterization.

Could use a flow through centrifuge (biodiesel type) prior to filtration but I think that is most likely not the most efficient way.
 
B

ButterCup

Member
Gray Wolf said:
Typically at 48 hours, they would be out of solution, but still suspended.

Try using a sock filter, with more surface area, or using a paint brush to keep brushing the accumulated was off the surface of the membrane filter, to keep the pores open.
Click to expand...

Thank you for the input. Thanks for the ideas. :thank you:

Previously when i winterized in small volume at -10f the lipids sat in the bottom. For some reason they are suspended in larger volume.
 
B

ButterCup

Member
thegreenman91 said:
Hey Grey Wolf... Is there a good centrifuge for our industry? The largest I can find is 6x 1000ml. Is there a centrifuge with a large sized single bucket design that could effectively be used for winterization.

Could use a flow through centrifuge (biodiesel type) prior to filtration but I think that is most likely not the most efficient way.
Click to expand...

I would be interested in that too.
 
Gray Wolf

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
thegreenman91 said:
Hey Grey Wolf... Is there a good centrifuge for our industry? The largest I can find is 6x 1000ml. Is there a centrifuge with a large sized single bucket design that could effectively be used for winterization.

Could use a flow through centrifuge (biodiesel type) prior to filtration but I think that is most likely not the most efficient way.
Click to expand...

Good question and idea! I'll run it by our biotech Pharmer Joe and report back.
 
H

HealthWeed

New member
Same here. Can't get anything to really float. It all seems to stay suspended throughout the solution. I am doing a 10:1 100% ETOh soak for 48 hours @ -20C. I am then using a Whatman 1001 (11 micron) 125mm filter on a 125mm Buchner funnel setup. Any ideas as to why we can't get the lipids to float on top?
 
O

Old Gold

Active member
HealthWeed said:
Same here. Can't get anything to really float. It all seems to stay suspended throughout the solution. I am doing a 10:1 100% ETOh soak for 48 hours @ -20C. I am then using a Whatman 1001 (11 micron) 125mm filter on a 125mm Buchner funnel setup. Any ideas as to why we can't get the lipids to float on top?
Click to expand...
They shouldn't be floating on top of anything. They should drop to the bottom. Do you see anything fall at room temperature, when first dissolved?
Is the solution very hazy throughout and difficult to see through? If you don't have enough alcohol, they stay suspended throughout the solution, trapped with lots of cannibanoids as well. More ethanol might help give layers of separation and let waxes bind to one another better.
I'll upload a picture of waxes/lipids precipitating out of dark crude oil after only 24hrs in a -20C freezer.

picture.php
 
Last edited:
D

Digital Man

Member
Probably has to do with the intial extraction more than anything. I wouldn't be so concerned with what is looks like out of the freezer or how long it takes to filter out that quart of solution. As long as you have a fully winterized product at the end of the day what differnce does it make?
 
O

Old Gold

Active member
Digital Man said:
Probably has to do with the intial extraction more than anything. I wouldn't be so concerned with what is looks like out of the freezer or how long it takes to filter out that quart of solution. As long as you have a fully winterized product at the end of the day what differnce does it make?
Click to expand...

If the waxes are suspended throughout the solution, it warms as it runs through the filter, and nothing is getting left behind on top, I am gonna go ahead and guess that they aren't precipitating out and are passing through the filter in solution.
 
B

blastfrompast

Active member
Veteran
gotta KEEP everything cold when filtering.... So pouring cold solution over a warm filter and funnel could be your issue perhaps? Tho when buddy did this his buchi clogged with the waxes still but his filter paper didn't catch squat....
 
B

ButterCup

Member
I have a couple of ideas on why the lipids are staying suspended.

1. Could it be residual butane left in the oil?

2. Could using denatured alcohol (5% methanol or Iso) be causing problems.

I haven't been able to find a proper source for non-denatured alcohol in cali, so i opt for denatured with 5% methanol. When I add water to the denatured alcohol it turns cloudy which I was told was due to the presence of some ketone.
 
O

Old Gold

Active member
ButterCup said:
I have a couple of ideas on why the lipids are staying suspended.

1. Could it be residual butane left in the oil?

2. Could using denatured alcohol (5% methanol or Iso) be causing problems.

I haven't been able to find a proper source for non-denatured alcohol in cali, so i opt for denatured with 5% methanol. When I add water to the denatured alcohol it turns cloudy which I was told was due to the presence of some ketone.
Click to expand...

1. Super doubtful. You'd need a scary, visible quantity of liquid butane that should not be in a house or in a freezer.

2. No...... I use it all the time for winterization. Also, I get the cloudiness with it (water content) and not when I use acetone, which is the most simple ketone. I'll look up water solubilities. Is the denatured alcohol you use listed at 5% methanol in the safety data sheet or are you assuming?
 
E

easystephen

Member
What type of container are you using?

I actually try to avoid having the lipids and sugars crystalize on the container so that I don't have to clean it out every time. It also makes the process more efficient since I can pull the good stuff through the filtrate more effectively. We use HDPE jugs which tends to keep the filtrate floating rather than crystallized on the bottom of the container. When we have used glass beakers in the past, the sugars and lipids crystallize on the bottom.

It sounds like your real problem is not enough surface area on your filter. You should look at using a larger diameter filter, the surface area goes up like the square of the diameter so it makes a huge difference. Our 24" buchner has 450 sq in of surface area!
 
You must log in or register to reply here.

Latest posts

Latest posts

Top