Minimum Alcohol % Needed to Dissolve Cannabinoids

[Chris Edward]

Hello all,

Does anyone know the minimum alcohol content required to dissolve cannabinoids?

We all assume it’s 99%, right?

But people people use everclear all the time, which is an azeotrope of alcohol and water, 95:5.
This is strongest you can get alcohol by simple steam distillation. To go any higher requires the use of benzene, which causes cancer.

So, my question is, how low can you go?
I am certain 40% won't do it, but will 60%

I thought I would ask here before I did any of my own tests.

Thank you all in advance for your help...

 

[OPfarmer]

I see it as one wants the highest alcohol so you can evaporate it at lower than boiling water temps.

I use eveclear at 95% very effectively for quick sub zero washes and longer sub zero soaks.

Sounds like people have used 151 rum that's 75.5% quit successful. Also I believe many old school green dragon tinctures we're made with long soaks in plain old 40% vodka.

If you are try to make concentrates to dab or dose by weight is where I see the problem with higher water content.

Tinctures, maybe you have to drink a shot glass of vodka extracted stuff instead of a drop or two of concentrate.

Me I evaporate all the alcohol and water, to weigh accurately first then add alcohol back in for easy storage, handling and consumption.

 

[Chris Edward]

OPfarmer,
I am just curious.
I am thinking of making my own alcohol for extraction.
I use iso but I would prefer something that isn't a straight up poison.
I cannot buy everclear where I live and to have it delivered is crazy expensive.
I can buy all the equipment to make it myself for what a gallon of ethanol costs.
Plus I am not happy with the fact that in order to get 99% ethanol, they have to add benzene.

So, I am mostly just curious if something in the range of 80-95% is usable.
This is the range I can expect from simple home distillation.
And it's not like I need much, especially if I am able to reclaim like 80% of the alcohol through simple distillation.



There was a patent I was reading about where the company does this really neat trick. They extract the cannabis oil with 95:5 ethanol:water and then pass it through a system that adds water (but they don't say how much), diluting the alcohol and making it so the cannabis can "Fall out of solution."
The mixture is then put into containers and allowed to sit before some of the water:ethanol mixture is siphoned off, then what is left is frozen, so the cannabis oil rises to the top and semi freezes into a paste, which is then sort of lifted off the frozen water:ethanol solution, like taking fat off cold chicken soup.
The company then reclaims the ethanol by distillation.
Also apparently the water is retained and reused as well and what happens is after subsequent batches it begins to favor the chlorophyll and so despite a long extraction soaking period (which is a no-no for us normies), the chlorophyll is extracted as well.

The point of all of this hoo-haa is that their extraction method is completely contained and pretty safe.

Pretty interesting huh?

I found a really cool recipe on YouTube that uses sugar and bakers yeast to make vodka, so for like $15.00 I can make a gallon of distilled alcohol for use in extraction (I don't even need a quarter of that).
Compared to like $120 if I were to order it online.

How much do you pay for the everclear?
Just curious...

The highest alcohol we can get here is like 100 proof, which goes for like $30.00 for a 750ml bottle.

A few years ago it was either Tanqueray or Bombay gin that accidentally sent out bottles that were 95% but they quickly recalled them...
I don't think they reclaimed many, because the second folks heard about it, they bought as many as they could...LOL

 

[curious2garden]

OPfarmer,
I am just curious.
I am thinking of making my own alcohol for extraction.
I use iso but I would prefer something that isn't a straight up poison.
I cannot buy everclear where I live and to have it delivered is crazy expensive.
I can buy all the equipment to make it myself for what a gallon of ethanol costs.
Plus I am not happy with the fact that in order to get 99% ethanol, they have to add benzene.

So, I am mostly just curious if something in the range of 80-95% is usable.
This is the range I can expect from simple home distillation.
And it's not like I need much, especially if I am able to reclaim like 80% of the alcohol through simple distillation.



There was a patent I was reading about where the company does this really neat trick. They extract the cannabis oil with 95:5 ethanol:water and then pass it through a system that adds water (but they don't say how much), diluting the alcohol and making it so the cannabis can "Fall out of solution."
The mixture is then put into containers and allowed to sit before some of the water:ethanol mixture is siphoned off, then what is left is frozen, so the cannabis oil rises to the top and semi freezes into a paste, which is then sort of lifted off the frozen water:ethanol solution, like taking fat off cold chicken soup.
The company then reclaims the ethanol by distillation.
Also apparently the water is retained and reused as well and what happens is after subsequent batches it begins to favor the chlorophyll and so despite a long extraction soaking period (which is a no-no for us normies), the chlorophyll is extracted as well.

The point of all of this hoo-haa is that their extraction method is completely contained and pretty safe.

Pretty interesting huh?

I found a really cool recipe on YouTube that uses sugar and bakers yeast to make vodka, so for like $15.00 I can make a gallon of distilled alcohol for use in extraction (I don't even need a quarter of that).
Compared to like $120 if I were to order it online.

How much do you pay for the everclear?
Just curious...

The highest alcohol we can get here is like 100 proof, which goes for like $30.00 for a 750ml bottle.

A few years ago it was either Tanqueray or Bombay gin that accidentally sent out bottles that were 95% but they quickly recalled them...
I don't think they reclaimed many, because the second folks heard about it, they bought as many as they could...LOL

@cannabineer

 

[cannabineer]

OPfarmer,
I am just curious.
I am thinking of making my own alcohol for extraction.
I use iso but I would prefer something that isn't a straight up poison.
I cannot buy everclear where I live and to have it delivered is crazy expensive.
I can buy all the equipment to make it myself for what a gallon of ethanol costs.
Plus I am not happy with the fact that in order to get 99% ethanol, they have to add benzene.

So, I am mostly just curious if something in the range of 80-95% is usable.
This is the range I can expect from simple home distillation.
And it's not like I need much, especially if I am able to reclaim like 80% of the alcohol through simple distillation.



There was a patent I was reading about where the company does this really neat trick. They extract the cannabis oil with 95:5 ethanol:water and then pass it through a system that adds water (but they don't say how much), diluting the alcohol and making it so the cannabis can "Fall out of solution."
The mixture is then put into containers and allowed to sit before some of the water:ethanol mixture is siphoned off, then what is left is frozen, so the cannabis oil rises to the top and semi freezes into a paste, which is then sort of lifted off the frozen water:ethanol solution, like taking fat off cold chicken soup.
The company then reclaims the ethanol by distillation.
Also apparently the water is retained and reused as well and what happens is after subsequent batches it begins to favor the chlorophyll and so despite a long extraction soaking period (which is a no-no for us normies), the chlorophyll is extracted as well.

The point of all of this hoo-haa is that their extraction method is completely contained and pretty safe.

Pretty interesting huh?

I found a really cool recipe on YouTube that uses sugar and bakers yeast to make vodka, so for like $15.00 I can make a gallon of distilled alcohol for use in extraction (I don't even need a quarter of that).
Compared to like $120 if I were to order it online.

How much do you pay for the everclear?
Just curious...

The highest alcohol we can get here is like 100 proof, which goes for like $30.00 for a 750ml bottle.

A few years ago it was either Tanqueray or Bombay gin that accidentally sent out bottles that were 95% but they quickly recalled them...
I don't think they reclaimed many, because the second folks heard about it, they bought as many as they could...LOL

My reply will not be comprehensive.

One does not need benzene to make 99+% ethanol. Toluene will do, but the winning method is to vacuum distill wherein the azeotrope rises to 99.5% ethanol.

A decent (atmospheric) fractional distillation of oh, I dunno, vodka ... will yield 95% ethanol quite suitable for dissolving oleoresin Cannabis.

However I spent years learning the distiller's art. That Youtube recipe will probably do you a disservice if you don't have or want a good fractional still.

I imagine 90% or better ethanol:water will do just fine.

 

[Fadedawg]

OPfarmer,
I am just curious.
I am thinking of making my own alcohol for extraction.
I use iso but I would prefer something that isn't a straight up poison.
I cannot buy everclear where I live and to have it delivered is crazy expensive.
I can buy all the equipment to make it myself for what a gallon of ethanol costs.
Plus I am not happy with the fact that in order to get 99% ethanol, they have to add benzene.

So, I am mostly just curious if something in the range of 80-95% is usable.
This is the range I can expect from simple home distillation.
And it's not like I need much, especially if I am able to reclaim like 80% of the alcohol through simple distillation.



There was a patent I was reading about where the company does this really neat trick. They extract the cannabis oil with 95:5 ethanol:water and then pass it through a system that adds water (but they don't say how much), diluting the alcohol and making it so the cannabis can "Fall out of solution."
The mixture is then put into containers and allowed to sit before some of the water:ethanol mixture is siphoned off, then what is left is frozen, so the cannabis oil rises to the top and semi freezes into a paste, which is then sort of lifted off the frozen water:ethanol solution, like taking fat off cold chicken soup.
The company then reclaims the ethanol by distillation.
Also apparently the water is retained and reused as well and what happens is after subsequent batches it begins to favor the chlorophyll and so despite a long extraction soaking period (which is a no-no for us normies), the chlorophyll is extracted as well.

The point of all of this hoo-haa is that their extraction method is completely contained and pretty safe.

Pretty interesting huh?

I found a really cool recipe on YouTube that uses sugar and bakers yeast to make vodka, so for like $15.00 I can make a gallon of distilled alcohol for use in extraction (I don't even need a quarter of that).
Compared to like $120 if I were to order it online.

How much do you pay for the everclear?
Just curious...

The highest alcohol we can get here is like 100 proof, which goes for like $30.00 for a 750ml bottle.

A few years ago it was either Tanqueray or Bombay gin that accidentally sent out bottles that were 95% but they quickly recalled them...
I don't think they reclaimed many, because the second folks heard about it, they bought as many as they could...LOL

You can extract with brandy, and some brothers and sisters make canna liqueurs that way.

For concentrates, getting rid of the water later, usually leads extractors to start with a higher alcohol ratio. We typically use 190 proof/95% from the local liquor store @ about $48 per 1.5 liter.

For all of ya’ll living where 190 proof isn’t readily available, here are a couple sites that will ship most anywhere:

East coasters check out, http://www.winechateau.com/

West coasters, try http://organicalcohol.com/store/

A compound refluxing still will deliver a 95% azeotropic mixture at around $8/L and is easy to build. We used stainless pot scrubbers for the column packing.

https://web.archive.org/web/20150315114315/http://skunkpharmresearch.com/enabler-alcohol-fractionating-still/

The precise temperature feedback from the top of the column, will tell you what is coming out the top, so easy to tell at which points to pitch the "heads" with the methanol and ethyl acetate, as well when to shut off the "tails" to avoid the oils.

I would recommend using a distillers yeast, rather than bakers yeast, because it tolerates higher alcohol content before going dormant.

You can further dry the 190 proof if you desire, using Drierite, or Mol sieve instead of benzene. a vacuum still also moves the azeotrope balance closer to 100%.

Your technique using water recovery opens interesting questions regarding how undesirable water is for the initial extraction. If you run that experiment, I hope you share.

 

[OPfarmer]

Hard liquor is expensive in my state because of taxes. Everclear 750ml is $20 on sale.

I refuse to be poisoned by greedy f#$@& politicians, and use denatured ethanol.

In my condition I am not into DIY projects, was when I was younger though.

I bought a prepmade rig called the a "Source Turbo" extraction device. It's a vacuum chamber that gently heats the ethanol and reclaims it.

Making your own ethanol sure why not! Don't need to taste good. Simple enough to do, or you could distill cheap vodka too.

What is the final product you are trying to make?

IMHO Water in the ethanol only means you need to be patient evaporating it. Time is a small price to pay for piece of mind, by not using toxic chemicals.

 

[Thundercat]

I thought I posted this last night but I guess not.

I've made delicious tinctures with Makers Mark Whiskey, and I believe you can get some extraction in almost any alcohol. However how much you get obviously is subjective to how strong the alcohol is.

You NEVER want to use denatured alcohol!!!

Denatured and Isopropyl ARE NOT THE SAME THING!

Usually I use 91% Iso because its super cheap and very clean. With in 24 hours I've got a completely clean shatter style concentrate(usually shatter anyway). I've used Everclear, and it works great too, but is more expensive. Iso is fast, cheap, readily available, clean.............

If the OP is really into DIY then more power to doing your own distilling. I started to build a set up years ago to make some brandy but never followed through.

Honestly the idea of distilling alcohol just to do an extraction seems pretty over the top to me. I could never justify the time and money involved in the process of distilling for this intent. Distillation takes between days-weeks to get the kind of product you're looking for if you calculate in the brewing period for the mash. Then hours of distilling to get a small amount of alcohol.

 

[Chris Edward]

@cannabineer,

I know, but benzene is the most commonly used entrainer and I didn’t want to go listing all the non-polar solvents that could be used.

I figured if the alcohol needed to be higher than 95:5, I could always use a molecular sieve and then reclaim the sieve for regeneration and reuse later.

Fractional distillation is the route I am going to take.
I plan to include a bit of vacuum (venturi), to lower the boiling point a bit and allow the process to happen a bit quicker.

I went to the bakers yeast recipe after doing some research and finding out that while turbo yeast will produce a higher ABV wash (14%), the final distillate is basically jet fuel and must be filtered multiple times through carbon to smooth it out or else it is undrinkable because it is so harsh.
The bakers yeast recipe is supposed to take a bit longer (few days), and the wash will only be 10% compared to like 14% with turbo yeast, but the resulting vodka is much smoother without filtering.
Supposedly…
Not that I am going to be drinking the stuff.
The appeal of using simple and easily found ingredients is something I just cannot pass up.
Thank you for your help, I appreciate it.

 

[cannabineer]

@cannabineer,

I know, but benzene is the most commonly used entrainer and I didn’t want to go listing all the non-polar solvents that could be used.

I figured if the alcohol needed to be higher than 95:5, I could always use a molecular sieve and then reclaim the sieve for regeneration and reuse later.

Fractional distillation is the route I am going to take.
I plan to include a bit of vacuum (venturi), to lower the boiling point a bit and allow the process to happen a bit quicker.

I went to the bakers yeast recipe after doing some research and finding out that while turbo yeast will produce a higher ABV wash (14%), the final distillate is basically jet fuel and must be filtered multiple times through carbon to smooth it out or else it is undrinkable because it is so harsh.
The bakers yeast recipe is supposed to take a bit longer (few days), and the wash will only be 10% compared to like 14% with turbo yeast, but the resulting vodka is much smoother without filtering.
Supposedly…
Not that I am going to be drinking the stuff.
The appeal of using simple and easily found ingredients is something I just cannot pass up.
Thank you for your help, I appreciate it.

Yah the ternary drying additive I remember is toluene ... also effective and not as toxic.

I am curious though why you'd need an alcohol percentage above 95%.

As for yeast distillates ... what i have done with success is to treat the first-run distillate with a bit of lye. The next run is way smoother. YMMV.

In my opinion the bottleneck here is the still. I would not use a simple pot or kettle still. I'd see to having a fractional distillation capacity. My unit is Pyrex with an insulated helices-packed column. I have a stopcock on the condenser head that allows me (kludgily but still) to set a reflux ratio between column and receiver. Distillation is sort of a thing with me.

 

[Thundercat]

I meant to add I believe the number is 90% if you want to easily evap it afterward. Lower percentages will still extract but not as efficiently and the added water will make it take longer to evap.

 

[Chris Edward]

You can extract with brandy, and some brothers and sisters make canna liqueurs that way.

For concentrates, getting rid of the water later, usually leads extractors to start with a higher alcohol ratio. We typically use 190 proof/95% from the local liquor store @ about $48 per 1.5 liter.

For all of ya’ll living where 190 proof isn’t readily available, here are a couple sites that will ship most anywhere:

East coasters check out, http://www.winechateau.com/

West coasters, try http://organicalcohol.com/store/

A compound refluxing still will deliver a 95% azeotropic mixture at around $8/L and is easy to build. We used stainless pot scrubbers for the column packing.

https://web.archive.org/web/20150315114315/http://skunkpharmresearch.com/enabler-alcohol-fractionating-still/

The precise temperature feedback from the top of the column, will tell you what is coming out the top, so easy to tell at which points to pitch the "heads" with the methanol and ethyl acetate, as well when to shut off the "tails" to avoid the oils.

I would recommend using a distillers yeast, rather than bakers yeast, because it tolerates higher alcohol content before going dormant.

You can further dry the 190 proof if you desire, using Drierite, or Mol sieve instead of benzene. a vacuum still also moves the azeotrope balance closer to 100%.

Your technique using water recovery opens interesting questions regarding how undesirable water is for the initial extraction. If you run that experiment, I hope you share.

@Fadeddawg,

I was planning on using a fractionating distiller with vacuum and if need, also molecular sieve 3A to extract the water but leave the ethanol.

I do have concerns about using a “pot” still so while the modified BHO generator is cool, this would be a problem legally.
Lab-ware on the other hand sort of falls into a legal gray area.

As far as the heads and tails, I was thinking of just tossing the first 15%-20% of distillate and then doing a bulk distilling of about half the expected volume at which point I would then distill the remaining amount into various containers and place them in order to later be “analyzed” by smell.
Then the distillate that smells most like the initial bulk distillate will be retained and the remaining distillate will be saved for use as a cleaner/disinfector.

Thanks for the suggestion on the use of yeast, but I have done some research on bakers yeast and I believe it will work for my purposes.
10% washes will suit me just fine and I have no problem adding a few days to the ferment so the bakers yeast can get up to 8%-10%.

I would prefer to stay in the azeotrope range, because the alcohol will just revert back to this anyway, so why fight it…
As long as the cannabinoids dissolve in it, that’s all I can ask for, anything more would be just making life harder for no reason.


The idea I proposed isn’t mine, it was taken from a patent application.
US 2016/0228787 A1
It used to be that a patent application that sat for as long as this one would be considered DOA, but I have recently seen patents being granted on applications that are like 6 years old, so this could still be granted and then the patent would be in effect until 2035.

Seems like they are banking on it being granted because they have built an entire business around this idea, despite it’s “patent pending status” for the past 3.5+ years that the application has been sitting.

Here is their website:
https://www.escetllc.com/

There was a video on YouTube that went over the basics of the process but I cannot find it now.
Let me look around, I will find it.

I tried the technique with some olive oil dissolved in 99% iso alcohol.
Then I went through their general process.
The yield back was about 80% of the oil.
This was due to the fact that the sample was so small and the olive oil didn't really freeze, but turned into a paste.
I was trying to mimic my usual yield.
I assume if this were done in a continuous cycle with pounds of cannabis, the loss would be less and certainly less than what is lost due to current industry practices.
The only downside I found was that the amount of water needed to dilute the 99% iso so that the alcohol:water mixture would freeze was quite a bit of water. I suppose the amount of water doesn’t really matter because iso still boils at the same temperature no matter what volume of water it is in, except now it will be an azeotrope, which has a slightly different boiling point.

The beauty of this process is that the majority of it is entirely safe and it may be able to allow commercial cannabis extraction with a reduction regulations due to how safe the process is.
The only dangerous part is the alcohol extraction, which happens once, and is done in a closed loop, so there is nothing lost to the ambient air.
If a fire were to break out from this method, it could be extinguished quite easily.

I will look for the video and post a link when I find it.

Thanks for your input.

 

[Chris Edward]

Hard liquor is expensive in my state because of taxes. Everclear 750ml is $20 on sale.

I refuse to be poisoned by greedy f#$@& politicians, and use denatured ethanol.

In my condition I am not into DIY projects, was when I was younger though.

I bought a prepmade rig called the a "Source Turbo" extraction device. It's a vacuum chamber that gently heats the ethanol and reclaims it.

Making your own ethanol sure why not! Don't need to taste good. Simple enough to do, or you could distill cheap vodka too.

What is the final product you are trying to make?

IMHO Water in the ethanol only means you need to be patient evaporating it. Time is a small price to pay for piece of mind, by not using toxic chemicals.

@OPfarmer,

The Source Turbo looks pretty cool, it’s sort of a high tech “Super Flower Tower.”

This is very similar to the process of using an airstill, except the return on yield is 95% instead of 70-80% like with the air still.

The final product is going to be 20:1 CBD:THC, which I will then use as both a tincture and a vape.
I also recently got some CBD hemp seeds from a strain that is supposed to more bushy and less stalky than fiber hemp, so I am excited to try those out.
I have epilepsy and CBD helps reduce the frequency and the intensity of my seizures.
On CBD I can go up to 8-10 days without a seizure. Off it, I have a seizure every 3 to 4 days.


“Time is a small price to pay for piece of mind, by not using toxic chemicals.”
I couldn’t agree more…

Plus I am sort of geek when it comes to DIY, so I love making my own everything.
It really isn’t even about saving money, I just love the process.

 

[Chris Edward]

I thought I posted this last night but I guess not.

I've made delicious tinctures with Makers Mark Whiskey, and I believe you can get some extraction in almost any alcohol. However how much you get obviously is subjective to how strong the alcohol is.

You NEVER want to use denatured alcohol!!!

Denatured and Isopropyl ARE NOT THE SAME THING!

Usually I use 91% Iso because its super cheap and very clean. With in 24 hours I've got a completely clean shatter style concentrate(usually shatter anyway). I've used Everclear, and it works great too, but is more expensive. Iso is fast, cheap, readily available, clean.............

If the OP is really into DIY then more power to doing your own distilling. I started to build a set up years ago to make some brandy but never followed through.

Honestly the idea of distilling alcohol just to do an extraction seems pretty over the top to me. I could never justify the time and money involved in the process of distilling for this intent. Distillation takes between days-weeks to get the kind of product you're looking for if you calculate in the brewing period for the mash. Then hours of distilling to get a small amount of alcohol.

@Thundercat,

I would love to be able to use basic tinctures, but I am super sensitive to THC, so I have to know exactly how much I am working with so I can then dilute it down so the THC doesn’t trigger an anxiety attack.

To be honest the process of distilling is no more complicated than iso extraction, unless you are venting to open air (rice cooker), then that’s just reckless…
I don’t care how many times people claim to have done it “safely.”
Every time it this done this way they are rolling the dice and when the shit hits the fan with something like that, there is no time to think…
Ethanol gas is heavier than air, so it can pool in low spots like propane and when it goes up, it is fast, and super hot!!!

The total time to ferment and then distill an initial batch of ethanol takes about as long as making a tincture, but the yield from distillation and subsequent solvent recapture (95%+) will make it so you won’t have to make alcohol often.
The process of fractional distillation with vacuum assist is pretty fast, only a few hours from start to finished product.
Then it's just a matter of boiling off the remaining water.
Then you know exactly what you have and you can dilute it to the concentration you want.
That way there are no surprises.

I could go on about how Marker’s Mark (45% ABV) is like $22 for 750ml and how if you made it yourself it would only cost you $1.80 for the same amount of 45% alcohol.
Which you could then put into a canning jar with a calculated amount of charred white oak to age it.
But you have a process that works for you and as long as you are happy with it, why change it?
Right?

 

[Chris Edward]

Yah the ternary drying additive I remember is toluene ... also effective and not as toxic.

I am curious though why you'd need an alcohol percentage above 95%.

As for yeast distillates ... what i have done with success is to treat the first-run distillate with a bit of lye. The next run is way smoother. YMMV.

In my opinion the bottleneck here is the still. I would not use a simple pot or kettle still. I'd see to having a fractional distillation capacity. My unit is Pyrex with an insulated helices-packed column. I have a stopcock on the condenser head that allows me (kludgily but still) to set a reflux ratio between column and receiver. Distillation is sort of a thing with me.

@cannabineer,

Toulene is only “not as toxic” by theory, because there hasn’t been sufficient testing. For all we know it could be worse than benzene.
Plus “not as toxic” in chemistry is like saying sulfuric acid isn’t as strong as aqua regia…
They will both eat right through you…
Just one will dissolve your gold fillings as well…

As far as needing alcohol above 95%…
I don’t need it to be 95%…
My original post was about how low the percentage can go before the cannabinoids will no longer dissolve.

What spurred this post on was a YouTube video that I saw where a guy passed some cheap $10 a gallon wine (12% ABV) through an air still twice and came out with 85% alcohol.
So I was curious if between 70% and 85% ABV would dissolve cannabinoids.

Video #1:

Video #2:

I thought I would ask here first, before I did any tests just to see if anyone else knew.

As far as adding lye, is this used as a sanitizer?
Because I would doubt this is added to the ferment as the sodium would kill the yeast and I cannot see how hydrogen would be beneficial to the ferment either.
Nitrogen on the other hand, that would feed the yeast a bit.

I am with you on the still, it’s all glass for me too…
So all you’re missing is a rotary flask sitting in a heated bath and you’d have a rotovap, lol…

I am interested in the idea of setting the reflux ratio via stopcock, I have never heard of this…
I would be interested to hear more about this.

 

[Fadedawg]

@Fadeddawg,

I was planning on using a fractionating distiller with vacuum and if need, also molecular sieve 3A to extract the water but leave the ethanol.

I do have concerns about using a “pot” still so while the modified BHO generator is cool, this would be a problem legally.
Lab-ware on the other hand sort of falls into a legal gray area.

As far as the heads and tails, I was thinking of just tossing the first 15%-20% of distillate and then doing a bulk distilling of about half the expected volume at which point I would then distill the remaining amount into various containers and place them in order to later be “analyzed” by smell.
Then the distillate that smells most like the initial bulk distillate will be retained and the remaining distillate will be saved for use as a cleaner/disinfector.

Thanks for the suggestion on the use of yeast, but I have done some research on bakers yeast and I believe it will work for my purposes.
10% washes will suit me just fine and I have no problem adding a few days to the ferment so the bakers yeast can get up to 8%-10%.

I would prefer to stay in the azeotrope range, because the alcohol will just revert back to this anyway, so why fight it…
As long as the cannabinoids dissolve in it, that’s all I can ask for, anything more would be just making life harder for no reason.


The idea I proposed isn’t mine, it was taken from a patent application.
US 2016/0228787 A1
It used to be that a patent application that sat for as long as this one would be considered DOA, but I have recently seen patents being granted on applications that are like 6 years old, so this could still be granted and then the patent would be in effect until 2035.

Seems like they are banking on it being granted because they have built an entire business around this idea, despite it’s “patent pending status” for the past 3.5+ years that the application has been sitting.

Here is their website:
https://www.escetllc.com/

There was a video on YouTube that went over the basics of the process but I cannot find it now.
Let me look around, I will find it.

I tried the technique with some olive oil dissolved in 99% iso alcohol.
Then I went through their general process.
The yield back was about 80% of the oil.
This was due to the fact that the sample was so small and the olive oil didn't really freeze, but turned into a paste.
I was trying to mimic my usual yield.
I assume if this were done in a continuous cycle with pounds of cannabis, the loss would be less and certainly less than what is lost due to current industry practices.
The only downside I found was that the amount of water needed to dilute the 99% iso so that the alcohol:water mixture would freeze was quite a bit of water. I suppose the amount of water doesn’t really matter because iso still boils at the same temperature no matter what volume of water it is in, except now it will be an azeotrope, which has a slightly different boiling point.

The beauty of this process is that the majority of it is entirely safe and it may be able to allow commercial cannabis extraction with a reduction regulations due to how safe the process is.
The only dangerous part is the alcohol extraction, which happens once, and is done in a closed loop, so there is nothing lost to the ambient air.
If a fire were to break out from this method, it could be extinguished quite easily.

I will look for the video and post a link when I find it.

Thanks for your input.

The tax man wants his toll on drinking ethanol, and everyone should check their local regulations, but as you note, there is typically some wiggle room afforded to labs, as well as to stills with boilers under one gallon capacity for alcohol used in processes other than booze.

A simple pot still will take multiple runs to get above around 120 proof, so however you accomplish it, a refluxing column will get you there quicker. You can make the refluxing column out of a glass tube stuffed with stainless/copper wool, or attach a stainless or copper one to an all glass lab arrangement.

The beauty of having a thermometer at the top of a refluxing column, only the most concentrated vapors reach the column head, and a thermometer at that point will tell you exactly what boiling point vapors have reached there, so you can easily tell by the temperature reading exactly what is passing at that point, and when it is moving to the next lowest boiling point constituent.

Bread yeast works well, it just requires around double the amount of processing.

We typically use 190 proof as well, for most purposes. Why fight Mother Nature?

Thanks for the link and patent number! Doesn’t look like they want to share any process details on the site without first vetting the inquirer, but the patent looks interesting and I’ll check it out.

 

[OPfarmer]

Cool flower tower... But I don't have one.. this instead::

 

[Thundercat]

FYI @chrisedward I wasn't trying to poo on your idea. I think it's a noble endeavor. I think it would be a fun project to do this, as I mentioned before I have an appreciation for distillation.

My only hangups are the efficiency of the time and investment involved to produce a useable amount of alcohol. But I also live someplace where it's pretty easy to get everclear.

I would love to try one of the "source" units. I am curious though how hot it gets the solution. I do all my concentrate work with as little heat as possible. Even my evap never gets heated, it does a great job of retaining terps.

 

[Fadedawg]

@OPfarmer,

The Source Turbo looks pretty cool, it’s sort of a high tech “Super Flower Tower.”

This is very similar to the process of using an airstill, except the return on yield is 95% instead of 70-80% like with the air still.

The final product is going to be 20:1 CBD:THC, which I will then use as both a tincture and a vape.
I also recently got some CBD hemp seeds from a strain that is supposed to more bushy and less stalky than fiber hemp, so I am excited to try those out.
I have epilepsy and CBD helps reduce the frequency and the intensity of my seizures.
On CBD I can go up to 8-10 days without a seizure. Off it, I have a seizure every 3 to 4 days.


“Time is a small price to pay for piece of mind, by not using toxic chemicals.”
I couldn’t agree more…

Plus I am sort of geek when it comes to DIY, so I love making my own everything.
It really isn’t even about saving money, I just love the process.

We tested the Source Turbo and were impressed. Here is a link to that test: https://web.archive.org/web/20180407141510/https://skunkpharmresearch.com/extract-craft-source-turbo-ethanol-vacuum-recovery-unit/

We also tested the ISO-3 and 4, both of which also worked well. I note Wayback Machine didn't archive that one. They can also be used to reflux soxhlet material.

 

[cannabineer]

@cannabineer,

Toulene is only “not as toxic” by theory, because there hasn’t been sufficient testing. For all we know it could be worse than benzene.
Plus “not as toxic” in chemistry is like saying sulfuric acid isn’t as strong as aqua regia…
They will both eat right through you…
Just one will dissolve your gold fillings as well…

As far as needing alcohol above 95%…
I don’t need it to be 95%…
My original post was about how low the percentage can go before the cannabinoids will no longer dissolve.

What spurred this post on was a YouTube video that I saw where a guy passed some cheap $10 a gallon wine (12% ABV) through an air still twice and came out with 85% alcohol.
So I was curious if between 70% and 85% ABV would dissolve cannabinoids.

Video #1:

Video #2:

I thought I would ask here first, before I did any tests just to see if anyone else knew.

As far as adding lye, is this used as a sanitizer?
Because I would doubt this is added to the ferment as the sodium would kill the yeast and I cannot see how hydrogen would be beneficial to the ferment either.
Nitrogen on the other hand, that would feed the yeast a bit.

I am with you on the still, it’s all glass for me too…
So all you’re missing is a rotary flask sitting in a heated bath and you’d have a rotovap, lol…

I am interested in the idea of setting the reflux ratio via stopcock, I have never heard of this…
I would be interested to hear more about this.

I am a lab chemist by training, and I have a pretty fine gradation scale or sense for toxicity.

I am also a bit of a cowboy. I know how pretty much all the big bad ones smell. (Except dimethyl sulfate.) So I think of toluene, rightly or wrongly, as "will use" when benzene is on my Avoid list.

My gut call is that below 80% you'll have issues with solubility and possibly selectivity of extraction. I'd give 85% a try ... split the batch, extract one with 95% and the other with your waterier run ... weigh both solids and extract before and after. I'd use this gravimetric approach.

I added the sodium hydroxide (about 0.5% w/v) to the rather smelly first run of distillate and let it sit for a day before redistilling. It knocked out the yeasty fusely smells and flavors (yup, bioassay ftw!) and left me with a vodka-clean product.

As for describing fractional distillation in theory and practice, , that is a big subject that i bet Youtube has covered. But imo the two key components are a fractional distillation column and a distillation head with a thermometer port and a stopcock-controlled takeoff ratio (amount collected vs. amount returned back down the column). Here's a pic of the unit; it is similar to mine.