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"!

Vacuum distilling butane

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
For those of ya'll wishing to vacuum distill your butane to remove any heavier components, before using it for extraction, here is a design for the cold trap that we will be using as a test sled, to not only vacuum distill the butane, for further polish filtering it through a Bentonite, zeolite, etc, column.
The way it works, is that the butane is injected into the cold trap as a liquid and pumped off as a vapor, leaving behind those things with a higher boiling point.

I set my cold trap in 85F water. You can do it without setting the trap in warm water, but as the butane boils off under vacuum, the transition from liquid to vapor, liberates the heat of vaporization, and plunges the temperature of the pool of butane to below its boiling point, so the process moves in starts and stops.

The next Alkane boils at about 36.1C/98.6F, at atmospheric pressure, so it is important to not heat the pot much beyond about 85F. The thermometer in the cold trap lid will tell you at what temperature your butane pool is during the cycle.

It is also important to not recover the butane below where the compound pressure gauge reads zero pressure, zero vacuum, or 14.7 PSIA.

PSIA is pounds per square inch absolute, which starts at absolute zero, without the weight of the atmosphere (at full vacuum). The atmosphere weighs 14.7 pounds per square inch, which is what a 1" column of mercury 29.92" tall weighs.

We do this operation outside and recommend that everyone do the same. Even though it is ostensibly a fully enclosed system, what if there is a leak or something goes wrong, goes wrong, goes wrong..........?

I recommend that you read and heed the thread on Butane Safety, before embarking on this journey. http://skunkpharmresearch.com/butane-safety/

Pull a full vacuum on the empty 50# refrigerant recovery tank for the first time, and valve it off.

Attach the pressure gauge to the cold trap via 1/4" refrigerant hose and pull a full vacuum on the trap, and valve it off, before assembling the system.

To vacuum distill using the cold trap, attach a 1/4" refrigerant hose to the inlet of the cold trap, and the other end to either an LP-5 tank of n-Butane, or to a can tapper, preferably with a ball valve attached at the tapper.

Attach the 1/2" outlet hose to the top of the filter section and the other end goes to the inlet of a refrigerant recovery pump.

We've used a couple of inexpensive brands for this purpose, namely the Appion G-5 twin and the CPS T-21, but neither are not rated by the manufacturer for butane, because they are not explosion proof should a leak occur.

Our larger commercial sized Mk V Terpenator will have the more expensive Caresaver Universal, or a Haskell pneumatic refrigerant recovery pump as an option, that are rated for flammable refrigerants, such as R-600 (n-Butane).
Depending on your situation, you should pick an option that fits your needs and safety needs.

The other hose goes to the red liquid dip tube valve on the 50# refrigerant recovery tank, which is sitting in an ice bath. If you really want to fly, set it in a denatured alcohol bath, with chunks of dry ice dropping the temperature to -70F or so.

Start the refrigerant recovery pump and the open the red valve on the refrigerant recovery tank, as well as the outlet valve on the cold trap.

If you are using an LP-5 tank of n-Butane, set the tank on a refrigerant scale and weigh it. Record the weight and push tare on the scale.

Open the inlet valve on the cold trap slowly and transfer about two liters of butane, or about 1146 grams, 2.5 lbs. Close the inlet valve.

The pressure gauge will have gone from -29.92" Hg vacuum, to positive pressure in the range of 10 to 30 psi. Watch until the pressure gauge drops to zero pressure, zero vacuum, and then load another 2 liters for distillation.

If you are using canned butane and a can tapper, close the valve at the can tapper, and open the inlet valve on the trap fully.

Tap the can and open the ball valve at the tapper. The pressure will rise from zero, to positive pressure. When the recovery pump lowers the pressure back to zero pressure, zero vacuum, close the valve at the tapper and tap a new can.

Open the valve to drain that can as well, and continue this cycle until all cans are empty.

Once you have emptied the LP-5 or the cans, when the pressure reaches zero again, close all valves and turn off the recovery pump.

Disconnect the hoses from the trap and open all valves to let it breath.

Remove the lid to the cold trap to remove the materials removed from the butane, and clean the trap with denatured alcohol for the next batch of butane.
 

Attachments

  • BHO Cold Trap assy detail-1-1.jpg
    BHO Cold Trap assy detail-1-1.jpg
    27.6 KB · Views: 15

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Could someone clear the propane in a standard five gallon BBQ grill propane tank of ethanethiol (mercaptan/odorant) along with any other residues with this method? Ethanethiol's boiling point is 95F, http://en.wikipedia.org/wiki/Ethanethiol

Those that I'm aware of trying, were unsuccessful. They are detectable by taste and smell into the low parts per billionth.
 

Crunchnasty13

New member
I am interested in this, because it makes things cleaner, but it seems a little complex.... can you show an instructional for new guys? I wouldn't know where to start, from buying the parts, to assembling it, and running etc.
 

Hash Man

Member
Graywolf- Can I just do an empty run through my extracter and recover the butane, and then clean out my collection pot or must i build a seperate cold trap?
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Graywolf- Can I just do an empty run through my extracter and recover the butane, and then clean out my collection pot or must i build a seperate cold trap?

You can do the same thing with a Terpenator, if you already have one. This is a slightly cheaper alternative for those whom do not.
 

Crunchnasty13

New member
Can you remove the unwanted propane/random gasses from canned butane in addition to the oils and waxes that are undesirable? Basically turning canned butane into n-tane?

I've read that the propane has a higher psi, so it causes problems in the recovery process.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Can you remove the unwanted propane/random gasses from canned butane in addition to the oils and waxes that are undesirable? Basically turning canned butane into n-tane?

I've read that the propane has a higher psi, so it causes problems in the recovery process.

Yes you could fractionally distill off the Iso and Propane, but they do a good extraction job, and if you take them away, you will be paying a lot for your n-Butane. Probably cheaper to just buy n-Butane.

Propane doesn't cause problems for a powered recovery system, though it takes longer that butane to recover.

You can burp it off from a passive system, if you chill the tank to below -11C/10F and open the vapor valve.

You can burp off the Iso and Propane by chilling the tank to 20F or so, so that the n-Butane is in stable liquid state and opening the vapor valve.
 

Crunchnasty13

New member
I just emailed Dave from Tamisium, he denied that contaminants exist in the butane... maybe he doesn't understand what I'm talking about? He said they are just rumors from people to cause fear etc.
 

Crunchnasty13

New member
Ok... I was interested in a powered recovery system, but it looks like hit and miss when trying to get a unit from specializedformulations.com - there isn't any info on the site about the units themselves either, just a number and email. The equipment is all on backorder or out of stock.

I'm looking for a unit that isn't too complex, that can run up to 1lb (16oz) in a decent amount of time. Any suggestions? If so, do you have a link to any threads that show the step by step of how it's supposed to be operated?

If I know exactly what I need, I'd feel more comfortable contacting them about it, since it looks like that's how it needs to be.

Does their equipment have a nozzle adapter for cans? Tapping into them seems foolish.
 

Crunchnasty13

New member
Also, you gave me two temperature ranges - below 10F, and around 20F for burping off the iso and propane...I don't understand which one to use. Is one temp for a passive system, and the other temp for something else?
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
BHO remains constantly under attack by detractors, some of which lie like a rug and also post on this forum, so Dave from Tamisium is probably is reacting without checking out the new facts. Understandable, but to his discredit, not a good thing in this case.

Isobutane boils at about 11F, so you must be below that temperature to keep from boiling it off. You can burp the propane at 20 to 30F, as n-Butane boils around 30.5F.

Foolish or not, the can tapper has proven to be the best solution yet to remove the contents without a bunch of accompanying air, or releases to atmosphere. In the refrigeration business, any VOC releases to atmosphere are not tolerated.

Lots of information on Terpenators on the Skunkpharmresearch.com site. I recommend that you start there.

A Mk I or II will hold one to two pounds, depending on column. Not sure what the BHOgart's hold, but bet Matt would be willing to fill you in, if you contact him.

Yeah, the Terpenators have gone viral and Glacier Tank hasn't been able to keep up with the parts demand. I had to special order the last set of 12" X 12" sanitary spools from China, because the stock ones were all gone as soon as they arrived. Mostly purchased by Specialized Formulations

On the other hand, until you get your name on a waiting list, the parts situation isn't likely to improve soon.

A stellar alternative, is just to build your own. The parts are are available elsewhere, for substantially more money, and if you built it your self, the savings in markup and labor might make up most of the difference.
 

BagAppeal

Member
Dear Gray Wolf

What are your thoughts on doing a fractional distillation, compared to a average vaacum?
Would it be possible to separate components within the bho?
Hope i am not to much off topic.

All the best
BagAppeal
 
Wow gray wolf. You understand how to scfe and you encourage butane as a solvent of choice isn't kosher. I recently beat manufacturing charges on my own knowledge of the law and a statement proving legitimacy and ultimately DA Rejected case. I have no bar membership yet represented myself like a big boy not only by copping it was mine, but what its legitamate use is in an andustry where I am trying to help correct is the bho being to tempermental, fast spreading, unnecessary methods that cost people their lives.BHO is gave hash oil a rael bad name
 
I was looking @ 8 years because of stupid irresponsable people having structural fires and not knowing what to do. This whole thing looks complicating w the beast still not being tame. When I can't afford ethanol, isobutane is the next affordable co-solvent. I can extract w a candle near a foot away and not have the extract ignite. My methods are supersimple solutions to supercritical fluids. The answer is really a subcritical liquid. Really the government yawns at hydrocarbon extractions, but look at supercritical co2 as way of the future. So I am venturing into subcritical water which is at 300 bar and 374C or 705F. As it is in more abundance than co2, leaves no residues, nor inherit tastes, seems to be the ultimate solvent of choice as its non-flammable as well.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Dear Gray Wolf

What are your thoughts on doing a fractional distillation, compared to a average vaacum?
Would it be possible to separate components within the bho?
Hope i am not to much off topic.

All the best
BagAppeal

Cannabis oil can be fractionally distilled, but it is above my pay grade. Joe, our biochemistry brain trust, is working on that issue, but alas is over the hill and far away, getting heart surgery for his last man child.

I will pick his keen alleged mind upon his return and get an update on his progress.

He has an open experiment using Chromatography to separate the components and light refraction to redirect the streams to different containers.

He picked up the used fractionator off e-bay, and you can see it in the background, behind the vacuum distillation experiment.
 

Attachments

  • Fractionator-1-1.jpg
    Fractionator-1-1.jpg
    64.5 KB · Views: 13

Latest posts

Latest posts

Top